Accessing osmium(VI) nitrido complexes with N-heterocyclic carbene ligands.
Parche, Joshua; Sievers, Robin; Streit, Tim-Niclas; Malischewski, Moritz; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5161–5167; doi:10.1039/d6dt00234j

data_7720358
_publ_section_title
;
 Accessing osmium(VI) nitrido complexes with N-heterocyclic carbene
 ligands.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5161
_journal_page_last               5167
_journal_paper_doi               10.1039/d6dt00234j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C42 H44 Cl7 N5 Os, 3(C H2 Cl2)'
_chemical_formula_sum            'C45 H50 Cl13 N5 Os'
_chemical_formula_weight         1311.95
_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     iterative
_audit_creation_date             2026-01-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2026-01-27 deposited with the CCDC.	2026-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.471(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5753(14)
_cell_length_b                   12.4895(8)
_cell_length_c                   22.0707(17)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.483
_cell_measurement_theta_min      2.353
_cell_volume                     5278.0(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.460
_diffrn_reflns_theta_min         2.127
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0903 after correction.
The Ratio of minimum to maximum transmission is 0.6691.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.996
_exptl_crystal_size_mid          0.427
_exptl_crystal_size_min          0.408
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.153
_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     590
_refine_ls_number_reflns         10927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0667P)^2^+7.6075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8989
_reflns_number_total             10927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00234j2.cif
_cod_data_source_block           p21n_twin_a
_cod_depositor_comments
'Adding full bibliography for 7720358--7720361.cif.'
_cod_database_code               7720358
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.148
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5542(15)
 0.4458(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C01H(H4,H), C01R(H5,Hi), C01S(H3,Hj)
3.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C016(H016), C017(H017), C018(H018), C01D(H01j), C01F(H01n),
 C01G(H01o), C01M(H01z)
3.c Idealised Me refined as rotating group:
 C00Y(H00a,H00b,H00c), C011(H01a,H01b,H01c), C015(H01d,H01e,H01f), C01A(H01g,
 H01h,H01i), C01E(H01k,H01l,H01m), C01I(H01p,H01q,H01r), C01J(H01s,H01t,H01u),
 C01K(H01v,H01w,H01x), C01L(H01y,Ha,Hb), C01N(H01,Hc,Hd), C01O(H1,He,Hf),
 C01Q(H2,Hg,Hh)
;
_shelx_res_checksum              90539
_olex2_exptl_crystal_mounting_method -
_olex2_submission_special_instructions 'No special instructions were received'