N Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Complexes of Molybdenum(IV) and Tungsten(IV)
Luz, Christian; Glok, Eduard; Horrer, Günther; Radius, Udo; Dalton Transactions  (2022) –; doi:10.1039/D2DT03409C

data_7711767
_publ_section_title
;
 N Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Complexes of
 Molybdenum(IV) and Tungsten(IV)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03409C
_journal_year                    2022
_chemical_formula_moiety         'C54 H72 Cl4 N4 W, C6 H6'
_chemical_formula_sum            'C60 H78 Cl4 N4 W'
_chemical_formula_weight         1180.91
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   47.1426(4)
_cell_length_b                   47.1426(4)
_cell_length_c                   13.96600(10)
_cell_measurement_reflns_used    85849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8420
_cell_measurement_theta_min      1.9510
_cell_volume                     26880.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66303
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.683
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             10944
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         14821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+63.9198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13842
_reflns_number_total             14821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03409c2.cif
_cod_data_source_block           compound_4
_cod_original_cell_volume        26880.0(5)
_cod_database_code               7711767
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.637
_shelx_estimated_absorpt_t_max   0.711
_shelx_res_checksum              76419
_shelx_hkl_checksum              57014