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_7711770
_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         'C42 H48 Cl4 N4 W, C6 H6'
_chemical_formula_sum            'C48 H54 Cl4 N4 W'
_chemical_formula_weight         1012.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                76.1480(10)
_cell_angle_beta                 81.7940(10)
_cell_angle_gamma                75.4250(10)
_cell_formula_units_Z            2
_cell_length_a                   12.51660(10)
_cell_length_b                   12.61370(10)
_cell_length_c                   15.29640(10)
_cell_measurement_reflns_used    82095
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.7520
_cell_measurement_theta_min      2.1860
_cell_volume                     2260.55(3)
_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      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1157
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            94116
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.943
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.115
_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     526
_refine_ls_number_reflns         9248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+1.3617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9002
_reflns_number_total             9248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03409c2.cif
_cod_data_source_block           compound_3
_cod_database_code               7711770
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              36872
_shelx_hkl_checksum              12619