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_7720359
_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 Cl4 N14 Os, 3(C4 H8 O)'
_chemical_formula_sum            'C54 H68 Cl4 N14 O3 Os'
_chemical_formula_weight         1293.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 108.1210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7601(9)
_cell_length_b                   11.7745(5)
_cell_length_c                   20.9785(9)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.326
_cell_measurement_theta_min      2.197
_cell_volume                     6047.4(4)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         2.197
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.079
_refine_diff_density_max         2.196
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5729
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0635P)^2^+87.5128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5209
_reflns_number_total             5729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00234j2.cif
_cod_data_source_block           c2_c_twinnniiii_niklas
_cod_depositor_comments
'Adding full bibliography for 7720358--7720361.cif.'
_cod_database_code               7720359
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.783(3)
 0.217(3)
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. Restrained distances
 O2-C3 = O2-C6
 1.44 with sigma of 0.02
 C3-C4 = C5-C6
 1.53 with sigma of 0.02
 C4-C5
 1.54 with sigma of 0.02
 O2-C4 = O2-C5 = C3-C5 = C4-C6
 2.38 with sigma of 0.04
 C3-C4 \\sim C4-C5 \\sim C5-C6
 with sigma of 0.02
 O2-C3 \\sim O2-C6
 with sigma of 0.02
 O2-C4 \\sim O2-C5
 with sigma of 0.04
 C4-C6 \\sim C3-C5
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C00Y(0.75) H00W(0.75) H00X(0.75) O00Z(0.75) C011(0.75) H01A(0.75)
 H01B(0.75) C012(0.75) H01C(0.75) H01D(0.75) C014(0.75) H01E(0.75) H01F(0.75)
 O2(0.75) C3(0.75) H3A(0.75) H3B(0.75) C4(0.75) H4A(0.75) H4B(0.75) C5(0.75)
 H5A(0.75) H5B(0.75) C6(0.75) H6A(0.75) H6B(0.75)
7.a Secondary CH2 refined with riding coordinates:
 C00Y(H00W,H00X), C011(H01A,H01B), C012(H01C,H01D), C014(H01E,H01F), C3(H3A,
 H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
7.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00M(H00M), C00U(H00U)
7.c Idealised Me refined as rotating group:
 C00H(H00A,H00B,H00C), C00O(H00D,H00E,H00F), C00S(H00G,H00H,H00J), C00V(H00L,
 H00N,H00O), C00W(H00P,H00Q,H00R), C00X(H00S,H00T,H00V)
;
_shelx_res_checksum              14405
_olex2_exptl_crystal_mounting_method -
_olex2_submission_special_instructions 'No special instructions were received'