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_1562894
_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         'C26 H16 Cl2 N2 O2 Os'
_chemical_formula_sum            'C26 H16 Cl2 N2 O2 Os'
_chemical_formula_weight         649.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 95.607(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.961(3)
_cell_length_b                   19.454(7)
_cell_length_c                   16.217(6)
_cell_measurement_reflns_used    287
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.85
_cell_measurement_theta_min      2.44
_cell_volume                     2185.6(15)
_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 0.990
_diffrn_measured_fraction_theta_max 0.985
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.1504
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5808
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.639
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.108
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/2 (Bruker,2010) was used for absorption correction.

Final HKLF 4 output contains 27519 reflections, Rint = 0.2006
 (2557 with I > 3sig(I), Rint = 0.0597)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.939
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0315P)^2^+15.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3768
_reflns_number_total             5808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00695a2.cif
_cod_data_source_block           Os8
_cod_depositor_comments
'Adding full bibliography for 1562893--1562894.cif.'
_cod_original_cell_volume        2185.4(14)
_cod_database_code               1562894
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.310
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7888(15)
 0.2112(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              70795
_olex2_submission_special_instructions 'No special instructions were received'