Double donation in trigonal planar iron-carbodiphosphorane complexes - a concise study on their spectroscopic and electronic properties.
Kneusels, Nis-Julian H; Münzer, Jörn E; Flosdorf, Kimon; Jiang, Dandan; Neumüller, Bernhard; Zhao, Lili; Eichhöfer, Andreas; Frenking, Gernot; Kuzu, Istemi; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2537–2546; doi:10.1039/c9dt04725e

data_7703463
_publ_section_title
;
 Double donation in trigonal planar iron-carbodiphosphorane complexes - a
 concise study on their spectroscopic and electronic properties.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2537
_journal_page_last               2546
_journal_paper_doi               10.1039/c9dt04725e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C39 H62 Fe N2 P2 Si4'
_chemical_formula_sum            'C39 H62 Fe N2 P2 Si4'
_chemical_formula_weight         789.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-13
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-17 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3110(8)
_cell_length_b                   16.4794(7)
_cell_length_c                   21.9452(10)
_cell_measurement_reflns_used    29797
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.23
_cell_volume                     4452.2(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL 2014/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29404
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.949
_diffrn_reflns_theta_min         2.264
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.8731
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XRED32
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       octahedra
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.493
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3710 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         10570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                9194
_reflns_number_total             10570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04725e2.cif
_cod_data_source_block           p212121
_cod_depositor_comments
'Adding full bibliography for 7703461--7703463.cif.'
_cod_database_code               7703463
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              17796
_olex2_submission_special_instructions 'No special instructions were received'