Metallocenium incorporated charge-enhanced thiourea catalysts
Blechschmidt, Daniel R.; Mergendahl, Cal; Kass, Steven R.; Organic & Biomolecular Chemistry 22 (2024) 1788–1793; doi:10.1039/D3OB02007J

data_7159795
_publ_section_title
;
 Metallocenium incorporated charge-enhanced thiourea catalysts
;
_journal_issue                   9
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1788
_journal_page_last               1793
_journal_paper_doi               10.1039/D3OB02007J
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C17 H16 Co F6 N2 P S'
_chemical_formula_sum            'C17 H16 Co F6 N2 P S'
_chemical_formula_weight         484.28
_chemical_melting_point          162(3)
_chemical_name_common            'cobaltocenium thiourea hexafluorophosphate'
_chemical_name_systematic
'N-Cobaltocenium-N'-phenylthiourea hexafluorophosphate'
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2024-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9480(4)
_cell_length_b                   13.3446(5)
_cell_length_c                   27.6271(9)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.18
_cell_volume                     3667.6(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0495
_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       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34402
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.513
_diffrn_reflns_theta_min         2.122
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.8658
_exptl_transmission_factor_min   0.8351
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
; 
 Flack x determined using 3627 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   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         11142
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.5531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                9617
_reflns_number_total             11142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob02007j2.cif
_cod_data_source_block           mo_19157_0m_a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_chemical_melting_point' value '159.8 -- 164.9' was
changed to '162(3)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7159795.cif.
;
_cod_database_code               7159795
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   'micro-focus sealed tube'
_shelx_res_checksum              15881
_shelx_hkl_checksum              72965