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_7708972
_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         'C13 H36 Co N2 O Si4, C18 H36 K N2 O6'
_chemical_formula_sum            'C31 H72 Co K N4 O7 Si4'
_chemical_formula_weight         823.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                111.7110(10)
_cell_angle_beta                 92.9320(10)
_cell_angle_gamma                108.9010(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5496(5)
_cell_length_b                   13.9247(6)
_cell_length_c                   15.1024(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.50
_cell_volume                     2275.40(16)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41838
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.082
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1085 before and 0.0511 after correction. The Ratio of minimum to maximum transmission is 0.9233. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       plank
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0328P)^2^+1.8172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7026
_reflns_number_total             9004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03924e3.cif
_cod_data_source_block           Co_CO_1_crypt
_cod_depositor_comments
'Adding full bibliography for 7708970--7708972.cif.'
_cod_database_code               7708972
_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:
 C23(H23A,H23B), C21(H21A,H21B), C27(H27A,H27B), C24(H24A,H24B), C28(H28A,
 H28B), C25(H25A,H25B), C22(H22A,H22B), C29(H29A,H29B), C14(H14A,H14B),
 C15(H15A,H15B), C20(H20A,H20B), C30(H30A,H30B), C31(H31A,H31B), C16(H16A,H16B),
  C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C),
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C4(H4A,
 H4B,H4C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.931