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_7704506
_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
'C27 H17 B Mo N3 O6 P6, C20 H40 Na O8, 2(C4 H8 O)'
_chemical_formula_sum            'C55 H73 B Mo N3 Na O16 P6'
_chemical_formula_weight         1347.72
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-06
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.824(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   29.5914(8)
_cell_length_c                   16.6475(5)
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    107(6)
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_cell_measurement_theta_min      3.1220
_cell_volume                     6382.1(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      107(6)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
  1 omega  -20.00   13.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -99.0000   60.0000 33

  2 omega   -3.00   45.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  -90.0000 48

  3 omega  -52.00   32.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -38.0000 -120.0000 84

  4 omega    4.00   84.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000 -180.0000 80

  5 omega  -52.00   30.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -77.0000  120.0000 82
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      0.0495903000
_diffrn_orient_matrix_UB_12      -0.0022122000
_diffrn_orient_matrix_UB_13      0.0181421000
_diffrn_orient_matrix_UB_21      -0.0227799000
_diffrn_orient_matrix_UB_22      -0.0005563000
_diffrn_orient_matrix_UB_23      0.0384980000
_diffrn_orient_matrix_UB_31      -0.0040683000
_diffrn_orient_matrix_UB_32      -0.0238576000
_diffrn_orient_matrix_UB_33      -0.0025985000
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99123
_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_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_preparation       '[MesMo(CO)] and PhB(OL)3Na in THF'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         14875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+27.4320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10703
_reflns_number_total             14875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           phbmoco3
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704506
_chemical_oxdiff_formula         Mo1B1P6C40H40N3O3
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14S(H14A,H14B), C23S(H23A,H23B), C25S(H25A,H25B), C22S(H22A,H22B), C26S(H26A,
 H26B), C18S(H18A,H18B), C27S(H27A,H27B), C24S(H24A,H24B), C15S(H15A,H15B),
 C13S(H13A,H13B), C17S(H17A,H17B), C28S(H28A,H28B), C20S(H20A,H20B), C21S(H21A,
 H21B), C19S(H19A,H19B), C16S(H16A,H16B), C12S(H12A,H12B), C8S(H8SA,H8SB),
 C9S(H9SA,H9SB), C4S(H4SA,H4SB), C7S(H7SA,H7SB), C1S(H1SA,H1SB), C11S(H11A,
 H11B), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB),
 C10S(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C5B(H5B), C4B(H4B), C3(H3), C3A(H3A), C6B(H6B), C6C(H6C), C3C(H3C), C7(H7),
 C3B(H3B), C6A(H6A), C4A(H4A), C5C(H5C), C4C(H4C), C4(H4), C6(H6), C5(H5),
 C5A(H5A)
;
_shelx_res_checksum              93191
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'nylon tip'
_olex2_submission_original_sample_id RS7041
_olex2_submission_special_instructions 'No special instructions were received'