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_1566183
_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         'C48 H62 Fe2 N2 O4 P4'
_chemical_formula_sum            'C48 H62 Fe2 N2 O4 P4'
_chemical_formula_weight         966.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 116.026(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9732(9)
_cell_length_b                   9.7552(4)
_cell_length_c                   16.3655(9)
_cell_measurement_reflns_used    3705
_cell_measurement_temperature    108.9(3)
_cell_measurement_theta_max      30.6660
_cell_measurement_theta_min      3.1600
_cell_volume                     2291.5(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      108.9(3)
_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 0.904
_diffrn_measurement_details
;
  1 omega  -91.00  -36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303  -57.0000 -180.0000 55

  2 omega  -10.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303   38.0000  120.0000 42

  3 omega  -19.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990  -99.0000  -90.0000 87

  4 omega    5.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6990   57.0000   60.0000 90

  5 omega -102.00  -55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.2303 -179.0000   60.0000 47
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145979000
_diffrn_orient_matrix_UB_12      0.0694739000
_diffrn_orient_matrix_UB_13      0.0059681000
_diffrn_orient_matrix_UB_21      0.0231588000
_diffrn_orient_matrix_UB_22      -0.0100455000
_diffrn_orient_matrix_UB_23      0.0477250000
_diffrn_orient_matrix_UB_31      0.0411580000
_diffrn_orient_matrix_UB_32      -0.0189794000
_diffrn_orient_matrix_UB_33      -0.0035295000
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18259
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.696
_diffrn_reflns_theta_min         2.770
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         7614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5487
_reflns_number_total             7614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4-anti.cif
_cod_data_source_block           redone
_cod_database_code               1566183
_chemical_oxdiff_formula         Fe2C40H40P4N2O12
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H23(0.02) H9(0.019) H10(0.022) H11(0.022) H13(0.018) H22(0.021)
 H24(0.023) H14A(0.033) H14B(0.033) H14C(0.033) H4A(0.037) H4B(0.037)
 H4C(0.037) H6A(0.032) H6B(0.032) H6C(0.032) H21(0.027) H16(0.021) H20(0.027)
 H5A(0.033) H5B(0.033) H5C(0.033) H15A(0.03) H15B(0.03) H15C(0.03) H17A(0.033)
 H17B(0.033) H17C(0.033) H18A(0.038) H18B(0.038) H18C(0.038)
 Fixed X: H23(0.4806) H9(0.2019) H10(0.159) H11(0.1519) H13(0.2674)
 H22(0.6219) H24(0.3406) H14A(0.1422) H14B(0.2304) H14C(0.2009) H4A(0.1038)
 H4B(0.0071) H4C(0.0897) H6A(0.0687) H6B(-0.0164) H6C(0.0589) H21(0.5729)
 H16(0.1964) H20(0.397) H5A(0.0886) H5B(0.0125) H5C(0.1138) H15A(0.3625)
 H15B(0.3878) H15C(0.4028) H17A(0.3309) H17B(0.2756) H17C(0.2686) H18A(0.096)
 H18B(0.1004) H18C(0.0479)
 Fixed Y: H23(0.182) H9(0.4764) H10(0.2503) H11(0.1074) H13(0.6414)
 H22(0.1782) H24(0.182) H14A(0.7213) H14B(0.8122) H14C(0.7007) H4A(0.6911)
 H4B(0.6168) H4C(0.5487) H6A(0.3351) H6B(0.4162) H6C(0.355) H21(0.1775)
 H16(0.1989) H20(0.1798) H5A(0.5765) H5B(0.6464) H5C(0.706) H15A(0.5968)
 H15B(0.7133) H15C(0.5594) H17A(0.0996) H17B(-0.0082) H17C(-0.0101)
 H18A(0.0027) H18B(0.007) H18C(0.1227)
 Fixed Z: H23(0.5627) H9(0.7645) H10(0.7619) H11(0.6473) H13(0.6071)
 H22(0.5356) H24(0.4102) H14A(0.6329) H14B(0.6865) H14C(0.7378) H4A(0.314)
 H4B(0.2778) H4C(0.2654) H6A(0.3447) H6B(0.3439) H6C(0.4352) H21(0.3685)
 H16(0.4593) H20(0.2899) H5A(0.5122) H5B(0.425) H5C(0.4708) H15A(0.7972)
 H15B(0.7459) H15C(0.7282) H17A(0.5749) H17B(0.4993) H17C(0.5919) H18A(0.509)
 H18B(0.4153) H18C(0.4407)
;
_shelx_res_checksum              25514
_shelx_hkl_checksum              4728
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'