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_7704513
_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 Mo N3 O6 P6 Si, 3(C4 H8 O)'
_chemical_formula_sum            'C39 H41 Mo N3 O9 P6 Si'
_chemical_formula_weight         1005.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
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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
;
2016-07-19 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_a                   28.4804(10)
_cell_length_b                   18.1858(6)
_cell_length_c                   16.8840(4)
_cell_measurement_reflns_used    5430
_cell_measurement_temperature    106.48(14)
_cell_measurement_theta_max      23.7860
_cell_measurement_theta_min      2.9200
_cell_volume                     8744.9(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
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_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.48(14)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
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_diffrn_measurement_details
;
  1 omega  -70.00   12.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303   19.0000 -120.0000 82

  2 omega  -42.00   45.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990  -57.0000 -120.0000 87

  3 omega   46.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990 -144.0000 -122.0000 50

  4 omega   -3.00   62.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   77.0000   60.0000 65

  5 omega    1.00   99.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   38.0000 -120.0000 98
;
_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      0.0247434000
_diffrn_orient_matrix_UB_12      0.0043938000
_diffrn_orient_matrix_UB_13      -0.0010697000
_diffrn_orient_matrix_UB_21      -0.0027622000
_diffrn_orient_matrix_UB_22      0.0386780000
_diffrn_orient_matrix_UB_23      0.0026820000
_diffrn_orient_matrix_UB_31      0.0008114000
_diffrn_orient_matrix_UB_32      -0.0023517000
_diffrn_orient_matrix_UB_33      0.0419075000
_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  0.1278
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47716
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.805
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83782
_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    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0972
_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^)+(0.0188P)^2^+61.7095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5726
_reflns_number_total             6938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01864c2.cif
_cod_data_source_block           pmmm
_cod_depositor_comments
'Adding full bibliography for 7704506--7704517.cif.'
_cod_database_code               7704513
_chemical_oxdiff_formula         'Mo1 Si1 P6 N3 C40 H60 O9'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C31(H31A,H31B), C32(H32A,H32B), C30(H30A,H30B), C28(H28A,H28B), C33(H33A,
 H33B), C39(H39A,H39B), C36(H36A,H36B), C29(H29A,H29B), C38(H38A,H38B),
 C35(H35A,H35B), C34(H34A,H34B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C3(H3), C24(H24), C6(H6), C4(H4), C20(H20), C9(H9), C12(H12),
 C5(H5), C15(H15), C18(H18), C21(H21), C10(H10), C16(H16), C22(H22), C17(H17),
 C11(H11)
;
_shelx_res_checksum              41563
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'