Carbon monoxide-driven osmium catalyzed reductive amination harvesting WGSR power
Biriukov, Klim O.; Vinogradov, Mikhail M.; Afanasyev, Oleg I.; Vasilyev, Dmitry V.; Tsygankov, Alexey A.; Godovikova, Maria; Nelyubina, Yulia V.; Loginov, Dmitry A.; Chusov, Denis; Catalysis Science & Technology 11 (2021) 4922–4930; doi:10.1039/D1CY00695A

data_1562893
_publ_section_title
;
 Carbon monoxide-driven osmium catalyzed reductive amination harvesting
 WGSR power
;
_journal_issue                   14
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4922
_journal_page_last               4930
_journal_paper_doi               10.1039/D1CY00695A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C25 H28 Cl N O2 Os'
_chemical_formula_sum            'C25 H28 Cl N O2 Os'
_chemical_formula_weight         600.13
_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     dual
_audit_creation_date             2021-04-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-04-05 deposited with the CCDC.	2021-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.999(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4652(9)
_cell_length_b                   9.6082(9)
_cell_length_c                   24.647(3)
_cell_measurement_reflns_used    1552
_cell_measurement_temperature    120
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.69
_cell_volume                     2241.1(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12741
_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         27.000
_diffrn_reflns_theta_min         2.152
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.831
_exptl_absorpt_correction_T_max  0.0511
_exptl_absorpt_correction_T_min  0.0232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.4540.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0217P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3625
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00695a2.cif
_cod_data_source_block           Os12
_cod_depositor_comments
'Adding full bibliography for 1562893--1562894.cif.'
_cod_database_code               1562893
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.274
_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 Ternary CH refined with riding coordinates:
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C14(H14), C15(H15), C17(H17),
 C19(H19), C20(H20), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              58203
_olex2_submission_special_instructions 'No special instructions were received'