Synthesis and structure of early transition metal NHC complexes
Lorber, Christian; Vendier, Laure; Dalton Transactions  (2009) 6972–; doi:10.1039/b905056f

data_7001944
_publ_section_title
;
 Synthesis and structure of early transition metal NHC complexes
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              6972
_journal_paper_doi               10.1039/b905056f
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H48 Cl2 N4 V, 0.5(C7 H8)'
_chemical_formula_sum            'C38.5 H52 Cl2 N4 V'
_chemical_formula_weight         692.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2301(12)
_cell_length_b                   13.2393(11)
_cell_length_c                   42.922(3)
_cell_measurement_reflns_used    2624
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1595
_cell_measurement_theta_min      2.8219
_cell_measurement_wavelength     0.71073
_cell_volume                     7518.1(11)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      0.0523004169
_diffrn_orient_matrix_UB_12      0.0081682917
_diffrn_orient_matrix_UB_13      0.0026150845
_diffrn_orient_matrix_UB_21      -0.009217367
_diffrn_orient_matrix_UB_22      0.0042540931
_diffrn_orient_matrix_UB_23      0.0162264348
_diffrn_orient_matrix_UB_31      0.0073496459
_diffrn_orient_matrix_UB_32      -0.052777825
_diffrn_orient_matrix_UB_33      0.0017177398
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1283
_diffrn_reflns_av_unetI/netI     0.1705
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            55113
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7683
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.075
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                3679
_reflns_number_total             7683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905056f.txt
_cod_data_source_block           9
_cod_original_formula_sum        'C38.50 H52 Cl2 N4 V'
_cod_database_code               7001944