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_7720360
_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 Cl6 F N5 Os'
_chemical_formula_sum            'C42 H44 Cl6 F N5 Os'
_chemical_formula_weight         1040.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8661(10)
_cell_length_b                   14.6551(7)
_cell_length_c                   14.3853(6)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      24.983
_cell_measurement_theta_min      2.477
_cell_volume                     4188.1(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         2.233
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0991 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.6887.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method cooling
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.507
_refine_diff_density_min         -2.540
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0278P)^2^+51.6289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2724
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00234j2.cif
_cod_data_source_block           pccafull
_cod_depositor_comments
'Adding full bibliography for 7720358--7720361.cif.'
_cod_database_code               7720360
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.723
_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. Uiso/Uaniso restraints and constraints
Uanis(N007) = Uanis(N009)
Ueq(N009): fixed at 0.05 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C00C(H00d), C00G(H00G), C00J(H00J), C00L(H00L)
3.b Idealised Me refined as rotating group:
 C00A(H00a,H00b,H00c), C00N(H00e,H00f,H00h), C00P(H00i,H00k,H00m), C00R(H00n,
 H00o,H00p), C00S(H00q,H00r,H00s), C00T(H00t,H00u,H00v)
;
_shelx_res_checksum              27853
_olex2_exptl_crystal_mounting_method '- '
_olex2_submission_special_instructions 'No special instructions were received'