Public Sub AddOrgRelationship()

'load Robert Hernandez constituent record from sample data
Dim oCon As CRecord
Set oCon = New CRecord
oCon.Init REApplication.SessionContext
oCon.LoadByField uf_Record_CONSTITUENT_ID, 96

Dim lId As Long
lId = oCon.Fields(RECORDS_fld_ID)

'load AAA Concrete organization record
Dim oCon2 As CRecord
Set oCon2 = New CRecord
oCon2.Init REApplication.SessionContext
oCon2.LoadByField uf_Record_CONSTITUENT_ID, 163

Dim lID2 As Long
lID2 = oCon2.Fields(RECORDS_fld_ID)

Dim oOrgRel As COrganization2
Set oOrgRel = New COrganization2

With oOrgRel
   .Init REApplication.SessionContext
   .Fields(ORGANIZATION2_fld_CONSTIT_ID) = lId
   .Fields(ORGANIZATION2_fld_RELATION_ID) = lID2
   .Save
End With

oOrgRel.CloseDown
Set oOrgRel = Nothing
oCon2.CloseDown
Set oCon2 = Nothing
oCon.CloseDown
Set oCon = Nothing

End Sub

Additional related articles:
How do I write code that creates an organizational relationship on an individual, but is not reciprocated?

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