Bis[2-(pyrrol-2-ylmethyleneamino)-2'-methoxy-6,6'-dimethyl-1,1'-biphenyl-κ^2^<i>N,N</i>']bis(dimethylamido-κ<i>N</i>)vanadium(IV) toluene monosolvate
Wang, Qiuwen; Xiong, Yihan; Deng, Xuebin; IUCrData 1 (2016) x161421–; doi:10.1107/S2414314616014218

data_1544074
_publ_section_title
;
 Bis[2-(pyrrol-2-ylmethyleneamino)-2'-methoxy-6,6'-dimethyl-1,1'-biphenyl-\k^2^<i>N,N</i>']bis(dimethylamido-\k<i>N</i>)vanadium(IV)
 toluene monosolvate
;
_journal_coeditor_code           HG4012
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x161421
_journal_paper_doi               10.1107/S2414314616014218
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '[V (C2 H6 N)2 (C20 H19 N2 O)2] , C7 H8'
_chemical_formula_moiety         'C44 H50 N6 O2 V, C7 H8'
_chemical_formula_sum            'C51 H58 N6 O2 V'
_chemical_formula_weight         837.97
_chemical_name_systematic
;Bis[2-(pyrrol-2-ylmethyleneamino)-2'-methoxy-6,6'-dimethyl-1,1'-biphenyl-\k^2^<i>N,N</i>']bis(dimethylamido-\k<i>N</i>)vanadium(IV) toluene
monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1400(10)
_cell_length_b                   19.2980(15)
_cell_length_c                   19.4490(16)
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      72.30
_cell_measurement_theta_min      27.50
_cell_volume                     4556.5(6)
_computing_cell_refinement
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2009)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2009)
;
_computing_data_reduction
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2009)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2010)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49860
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         72.453
_diffrn_reflns_theta_min         3.226
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrystalClear-SM Expert</i>; Rigaku, 2009)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       prism
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3251 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.0028(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         8875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                8286
_reflns_number_total             8875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg4012sup1.cif
_cod_data_source_block           I
_cod_database_code               1544074
_cod_database_fobs_code          1544074
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.722
_shelx_hkl_checksum              76191
_shelx_res_checksum              70886