High-spin carbonyl complexes of iron(I) and cobalt(I).
Schneider, Christian; Guggolz, Lukas; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 51 (2021) 179–184; doi:10.1039/d1dt03924e

data_7708971
_publ_section_title
;
 High-spin carbonyl complexes of iron(I) and cobalt(I).
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              179
_journal_page_last               184
_journal_paper_doi               10.1039/d1dt03924e
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C25 H60 Fe K N2 O7 Si4'
_chemical_formula_sum            'C25 H60 Fe K N2 O7 Si4'
_chemical_formula_weight         708.06
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2021-06-30
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-07-01 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.923(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6181(5)
_cell_length_b                   19.9580(10)
_cell_length_c                   23.1156(12)
_cell_measurement_reflns_used    5698
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.020
_cell_measurement_theta_min      2.22
_cell_volume                     3975.4(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29271
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.071
_diffrn_reflns_theta_min         2.223
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0575 after correction. The Ratio of minimum to maximum transmission is 0.8908. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       needle
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6058
_reflns_number_total             7815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03924e3.cif
_cod_data_source_block           Fe-CO_2_18c6
_cod_depositor_comments
'Adding full bibliography for 7708970--7708972.cif.'
_cod_database_code               7708971
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C14(H14A,H14B), C17(H17A,H17B), C15(H15A,H15B), C21(H21A,
 H21B), C25(H25A,H25B), C22(H22A,H22B), C23(H23A,H23B), C20(H20A,H20B),
 C24(H24A,H24B), C19(H19A,H19B), C18(H18A,H18B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C5(H5A,H5B,H5C),
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C4(H4A,
 H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.750
_shelx_estimated_absorpt_t_max   0.930