1,3,4-Azadiphospholides as building blocks for scorpionate and bidentate ligands in multinuclear complexes.
Suter, Riccardo; Wagner, Mona; Querci, Lorenzo; Conti, Riccardo; Benkő, Zoltán; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8201–8208; doi:10.1039/d0dt01864c

data_7704509
_publ_section_title
;
 1,3,4-Azadiphospholides as building blocks for scorpionate and bidentate
 ligands in multinuclear complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8201
_journal_page_last               8208
_journal_paper_doi               10.1039/d0dt01864c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H12 N3 O4 P7'
_chemical_formula_sum            'C18 H12 N3 O4 P7'
_chemical_formula_weight         551.10
_chemical_melting_point          413
_chemical_name_systematic
'tris([1,3,4]azadiphospholo[1,2-a]pyridin-3-yl) phosphate'
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
;
2016-07-21 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
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_cell_angle_gamma                93.858(3)
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_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
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_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
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_diffrn_measurement_details
;
  1 omega  -23.00    8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   60.0000 31

  2 omega  -19.00    8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000 -180.0000 27

  3 omega  -24.00   15.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -90.0000 39

  4 omega   -3.00   94.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   38.0000   90.0000 97

  5 omega   42.00   90.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000  -30.0000 48

  6 omega    2.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000 -180.0000 89

  7 omega  -46.00   48.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -38.0000  -90.0000 94

  8 omega  -98.00  -32.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  179.0000    0.0000 66

  9 omega    1.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  -60.0000 90
;
_diffrn_measurement_device       'kappa-stage diffractometer'
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_diffrn_orient_matrix_UB_13      0.0348217000
_diffrn_orient_matrix_UB_21      0.0042603000
_diffrn_orient_matrix_UB_22      -0.0456469000
_diffrn_orient_matrix_UB_23      0.0233982000
_diffrn_orient_matrix_UB_31      0.0272550000
_diffrn_orient_matrix_UB_32      -0.0390092000
_diffrn_orient_matrix_UB_33      -0.0474045000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.6761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4093
_reflns_number_total             4678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           mw26
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_original_cell_volume        1144.80(9)
_cod_database_code               7704509
_chemical_oxdiff_formula         'P7 C50 H50 N2 O4'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O00E)
3. Others
 Sof(O0)=Sof(O00E)=Sof(O00K)=Sof(O00N)=Sof(P0)=1-FVAR(1)
 Sof(P1)=Sof(O3)=Sof(O2)=Sof(O4)=Sof(O1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C15(H15), C4(H4), C10(H10), C9(H9), C17(H17),
 C11(H11), C3(H3), C18(H18), C16(H16)
;
_shelx_res_checksum              22297
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'