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_7720361
_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 F3 N5 Os, C5 H12'
_chemical_formula_sum            'C47 H56 Cl4 F3 N5 Os'
_chemical_formula_weight         1079.96
_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             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                 93.164(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.030(4)
_cell_length_b                   14.421(3)
_cell_length_c                   16.435(4)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      20.816
_cell_measurement_theta_min      2.478
_cell_volume                     4740.1(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0976
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            80980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.855
_diffrn_reflns_theta_max         20.855
_diffrn_reflns_theta_min         2.037
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1528 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.6888.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         4984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+39.4633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4152
_reflns_number_total             4984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00234j2.cif
_cod_data_source_block           p21c_new
_cod_depositor_comments
'Adding full bibliography for 7720358--7720361.cif.'
_cod_original_cell_volume        4739.9(19)
_cod_database_code               7720361
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(C00E) = Uanis(C00M)
3.a Secondary CH2 refined with riding coordinates:
 C01L(H3,HG), C01M(H4,HH), C01O(H6,HK)
3.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00N(H00N), C00R(H00R), C00S(H00S), C013(H013), C01A(H01M),
 C01E(H01W), C01G(H01Z)
3.c Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00C), C00Z(H00D,H00E,H00F), C015(H01A,H01B,H01C), C016(H01D,
 H01E,H01F), C018(H01G,H01H,H01I), C019(H01J,H01K,H01L), C01B(H01N,H01O,H01P),
 C01C(H01Q,H01R,H01S), C01D(H01T,H01U,H01V), C01F(H01X,H01Y,H), C01H(H01,HA,HB),
  C01J(H1,HC,HD), C01K(H2,HE,HF), C01N(H5,HI,HJ)
;
_shelx_res_checksum              62468
_olex2_submission_special_instructions 'No special instructions were received'