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_7708970
_publ_section_title
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 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         '1(C4 Co1 O4), 1(C12 H24 K1 O6)'
_chemical_formula_sum            'C16 H24 Co K O10'
_chemical_formula_weight         474.43
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_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
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2021-07-01 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.8148(9)
_cell_length_b                   13.8148(9)
_cell_length_c                   9.9198(7)
_cell_measurement_reflns_used    6189
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.67
_cell_volume                     1639.54(19)
_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    'ShelXT (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.109
_diffrn_reflns_theta_min         2.667
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1746 before and 0.1028 after correction. The Ratio of minimum to maximum transmission is 0.4739. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1617
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0390P)^2^+1.0084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1507
_reflns_number_total             1617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03924e3.cif
_cod_data_source_block           K(18c6)_Co(CO)4_3
_cod_depositor_comments
'Adding full bibliography for 7708970--7708972.cif.'
_cod_original_cell_volume        1639.5(2)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7708970
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.745
_olex2_refinement_description
;
1. Others
 Fixed U13: Co1(0) K1(0) O1(0) C1(0)
 Fixed U23: Co1(0) K1(0) O1(0) C1(0)
 Fixed Uiso: H00A(0.024) H00B(0.024) H00C(0.024) H00D(0.024) H00E(0.023)
 H00F(0.023) H00G(0.025) H00H(0.025)
 Fixed X: Co1(0.333333) K1(0.333333) H00A(0.021528) H00B(-0.043566)
 H00C(0.337902) H00D(0.313905) H00E(-0.002823) H00F(0.087222) O1(0.333333)
 H00G(0.122563) H00H(0.144516) C1(0.333333)
 Fixed Y: Co1(0.666667) K1(0.666667) H00A(0.549916) H00B(0.496441)
 H00C(0.427681) H00D(0.331638) H00E(0.352531) H00F(0.414589) O1(0.666667)
 H00G(0.287419) H00H(0.364375) C1(0.666667)
 Fixed Z: H00A(0.914657) H00B(0.776121) H00C(0.661507) H00D(0.769344)
 H00E(0.825888) H00F(0.94356) H00G(0.816992) H00H(0.686533)
;
_olex2_submission_special_instructions 'No special instructions were received'