Anionic 1-Aza-3,4-diphospholides as redox active ligands
Suter, Riccardo; Gilliard, Robert J.; Iskandarov, Javad; Benkő, Zoltan; Wörle, Michael; Grützmacher, Hansjörg; Inorganica Chimica Acta 520 (2021) 120274–; doi:10.1016/j.ica.2021.120274

data_1566181
_publ_section_title
;
 Anionic 1-Aza-3,4-diphospholides as redox active ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120274
_journal_paper_doi               10.1016/j.ica.2021.120274
_journal_volume                  520
_journal_year                    2021
_chemical_formula_moiety         'C36 H52 N2 O2 P4'
_chemical_formula_sum            'C36 H52 N2 O2 P4'
_chemical_formula_weight         668.67
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.150(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1651(6)
_cell_length_b                   8.7775(4)
_cell_length_c                   31.4231(17)
_cell_measurement_reflns_used    5544
_cell_measurement_temperature    109.96(13)
_cell_measurement_theta_max      27.0210
_cell_measurement_theta_min      3.0150
_cell_volume                     3630.4(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      109.96(13)
_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 0.999
_diffrn_measurement_details
;
  1 omega  -16.00   18.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   90.0000 34

  2 omega   -6.00   92.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592    0.0000 -180.0000 98

  3 omega  -46.00   47.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -38.0000  150.0000 93

  4 omega  -25.00   20.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -60.0000 45

  5 omega  -91.00    0.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -57.0000  -60.0000 91

  6 omega  -98.00  -34.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904 -179.0000    0.0000 64

  7 omega  -45.00   11.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -84.0000    3.0000 56

  8 omega  -25.00   64.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -99.0000    0.0000 89

  9 omega  -22.00   95.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   19.0000  -60.0000 117

 10 omega    1.00   30.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000  150.0000 29
;
_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      0.0498211000
_diffrn_orient_matrix_UB_12      0.0054930000
_diffrn_orient_matrix_UB_13      0.0089060000
_diffrn_orient_matrix_UB_21      -0.0151821000
_diffrn_orient_matrix_UB_22      -0.0439248000
_diffrn_orient_matrix_UB_23      0.0177093000
_diffrn_orient_matrix_UB_31      0.0139006000
_diffrn_orient_matrix_UB_32      -0.0676093000
_diffrn_orient_matrix_UB_33      -0.0107899000
_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  0.1097
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            47637
_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         26.372
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93039
_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    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0878
_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^)+(0.0290P)^2^+1.9820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5851
_reflns_number_total             7413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2-rac.cif
_cod_data_source_block           ppppni
_cod_database_code               1566181
_chemical_oxdiff_formula         P4NiC40H40O12N2
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H9(0.026) H29(0.024) H28(0.027) H17A(0.037) H17B(0.037)
 H17C(0.037) H11(0.027) H34(0.027) H27(0.027) H31(0.024) H10(0.033) H16(0.024)
 H23A(0.04) H23B(0.04) H23C(0.04) H13(0.028) H32A(0.041) H32B(0.041)
 H32C(0.041) H24A(0.041) H24B(0.041) H24C(0.041) H22A(0.046) H22B(0.046)
 H22C(0.046) H33A(0.049) H33B(0.049) H33C(0.049) H18A(0.048) H18B(0.048)
 H18C(0.048) H15A(0.048) H15B(0.048) H15C(0.048) H36A(0.05) H36B(0.05)
 H36C(0.05) H4A(0.049) H4B(0.049) H4C(0.049) H35A(0.055) H35B(0.055)
 H35C(0.055) H6A(0.055) H6B(0.055) H6C(0.055) H5A(0.051) H5B(0.051) H5C(0.051)
 H14A(0.075) H14B(0.075) H14C(0.075)
 Fixed X: H9(0.3457) H29(1.0712) H28(1.041) H17A(0.5195) H17B(0.5845)
 H17C(0.4656) H11(0.1931) H34(0.6508) H27(0.8768) H31(0.8872) H10(0.1986)
 H16(0.5867) H23A(0.8408) H23B(0.786) H23C(0.7768) H13(0.401) H32A(1.0114)
 H32B(1.0369) H32C(1.095) H24A(0.6405) H24B(0.7037) H24C(0.7588) H22A(0.5882)
 H22B(0.6086) H22C(0.5353) H33A(1.048) H33B(0.9938) H33C(0.9345) H18A(0.4931)
 H18B(0.6105) H18C(0.5431) H15A(0.3092) H15B(0.2792) H15C(0.2073) H36A(0.7191)
 H36B(0.6062) H36C(0.6882) H4A(0.633) H4B(0.5832) H4C(0.5151) H35A(0.698)
 H35B(0.6162) H35C(0.7309) H6A(0.6989) H6B(0.6819) H6C(0.7461) H5A(0.4401)
 H5B(0.505) H5C(0.5081) H14A(0.21) H14B(0.2758) H14C(0.3145)
 Fixed Y: H9(0.2846) H29(0.2396) H28(0.1553) H17A(-0.0024) H17B(-0.0021)
 H17C(0.0042) H11(0.3868) H34(0.1786) H27(0.1151) H31(0.3454) H10(0.3626)
 H16(0.2405) H23A(0.529) H23B(0.6875) H23C(0.5746) H13(0.3408) H32A(0.5099)
 H32B(0.4702) H32C(0.3882) H24A(0.4643) H24B(0.6153) H24C(0.4572) H22A(0.6215)
 H22B(0.7154) H22C(0.5748) H33A(0.1326) H33B(0.207) H33C(0.0924) H18A(0.2364)
 H18B(0.2411) H18C(0.3831) H15A(0.5699) H15B(0.4788) H15C(0.4774) H36A(0.1165)
 H36B(0.1506) H36C(0.2798) H4A(0.5149) H4B(0.6752) H4C(0.5288) H35A(-0.0728)
 H35B(-0.0714) H35C(-0.0982) H6A(0.6312) H6B(0.742) H6C(0.5931) H5A(0.5857)
 H5B(0.734) H5C(0.6057) H14A(0.194) H14B(0.1992) H14C(0.1083)
 Fixed Z: H9(0.1697) H29(0.4853) H28(0.5532) H17A(0.2291) H17B(0.1878)
 H17C(0.1842) H11(0.274) H34(0.5139) H27(0.5743) H31(0.407) H10(0.2013)
 H16(0.2196) H23A(0.4542) H23B(0.4521) H23C(0.4136) H13(0.3474) H32A(0.439)
 H32B(0.3918) H32C(0.4293) H24A(0.5246) H24B(0.5221) H24C(0.5204) H22A(0.4218)
 H22B(0.4635) H22C(0.4641) H33A(0.4034) H33B(0.3636) H33C(0.3922) H18A(0.1379)
 H18B(0.1474) H18C(0.1577) H15A(0.3416) H15B(0.3824) H15C(0.342) H36A(0.5981)
 H36B(0.5844) H36C(0.5824) H4A(0.2218) H4B(0.2286) H4C(0.2266) H35A(0.4985)
 H35B(0.5341) H35C(0.5462) H6A(0.3272) H6B(0.2886) H6C(0.283) H5A(0.2955)
 H5B(0.3019) H5C(0.3366) H14A(0.3395) H14B(0.3817) H14C(0.3422)
;
_shelx_res_checksum              31627
_shelx_hkl_checksum              72982
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'