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_1566182
_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         'C20 H26 Fe N O3 P2, C5 H5'
_chemical_formula_sum            'C25 H31 Fe N O3 P2'
_chemical_formula_weight         511.30
_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                 94.651(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6308(6)
_cell_length_b                   9.4136(4)
_cell_length_c                   16.6999(6)
_cell_measurement_reflns_used    2910
_cell_measurement_temperature    106.67(15)
_cell_measurement_theta_max      28.6640
_cell_measurement_theta_min      3.2550
_cell_volume                     2449.17(17)
_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      106.67(15)
_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
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -22.00   23.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -99.0000  120.0000 45

  2 omega    1.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   38.0000 -150.0000 89

  3 omega   -4.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   38.0000  120.0000 95

  4 omega  -50.00    2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -57.0000   60.0000 52
;
_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      -0.0186290000
_diffrn_orient_matrix_UB_12      -0.0001525000
_diffrn_orient_matrix_UB_13      -0.0401375000
_diffrn_orient_matrix_UB_21      0.0414667000
_diffrn_orient_matrix_UB_22      0.0050073000
_diffrn_orient_matrix_UB_23      -0.0141823000
_diffrn_orient_matrix_UB_31      0.0027587000
_diffrn_orient_matrix_UB_32      -0.0752190000
_diffrn_orient_matrix_UB_33      -0.0009098000
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11767
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.867
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84239
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_preparation       'FpI and 134ADP in thf'
_exptl_crystal_recrystallization_method 'Slow evaporation of DCM'
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.063
_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     296
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3624
_reflns_number_total             4316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           rs5074
_cod_original_cell_volume        2449.16(17)
_cod_database_code               1566182
_chemical_oxdiff_formula         C40H40P2N1O1Fe
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.026) H22(0.031) H9(0.026) H13(0.025) H16(0.027) H4A(0.038)
 H4B(0.038) H4C(0.038) H10(0.029) H21(0.029) H25(0.032) H6A(0.047) H6B(0.047)
 H6C(0.047) H24(0.035) H23(0.036) H15A(0.041) H15B(0.041) H15C(0.041)
 H5A(0.037) H5B(0.037) H5C(0.037) H18A(0.045) H18B(0.045) H18C(0.045)
 H14A(0.049) H14B(0.049) H14C(0.049) H17A(0.051) H17B(0.051) H17C(0.051)
 Fixed X: H11(0.8721) H22(0.617) H9(0.8077) H13(0.7507) H16(0.8216)
 H4A(0.9491) H4B(1.0211) H4C(0.9481) H10(0.8606) H21(0.4595) H25(0.4063)
 H6A(0.928) H6B(0.9968) H6C(0.9046) H24(0.5298) H23(0.6601) H15A(0.6223)
 H15B(0.6221) H15C(0.6406) H5A(0.8904) H5B(0.9849) H5C(0.9125) H18A(0.7706)
 H18B(0.7596) H18C(0.7059) H14A(0.7759) H14B(0.7588) H14C(0.8454) H17A(0.9635)
 H17B(0.9193) H17C(0.9275)
 Fixed Y: H11(0.0629) H22(0.5837) H9(0.4319) H13(0.6121) H16(0.16) H4A(0.3359)
 H4B(0.4132) H4C(0.3307) H10(0.2037) H21(0.5772) H25(0.3305) H6A(0.5591)
 H6B(0.6338) H6C(0.699) H24(0.1869) H23(0.3431) H15A(0.5018) H15B(0.6553)
 H15C(0.5238) H5A(0.697) H5B(0.6397) H5C(0.5581) H18A(-0.066) H18B(-0.0656)
 H18C(0.0395) H14A(0.6579) H14B(0.7776) H14C(0.6928) H17A(0.0999) H17B(-0.0236)
 H17C(-0.0325)
 Fixed Z: H11(0.554) H22(0.1078) H9(0.6504) H13(0.4673) H16(0.3496)
 H4A(0.4024) H4B(0.3589) H4C(0.3085) H10(0.6648) H21(0.1283) H25(0.0938)
 H6A(0.2304) H6B(0.2896) H6C(0.2747) H24(0.0528) H23(0.0621) H15A(0.4914)
 H15B(0.5278) H15C(0.5842) H5A(0.4231) H5B(0.4316) H5C(0.4722) H18A(0.4476)
 H18B(0.3535) H18C(0.4022) H14A(0.6352) H14B(0.5706) H14C(0.5755) H17A(0.3989)
 H17B(0.3479) H17C(0.442)
;
_shelx_res_checksum              13372
_shelx_hkl_checksum              77012
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'