Preparation and crystal structure of a non-symmetrical vanadium(II) dimer: tri-μ2-bromido-(hydrogen-tris(3-isopropyl-4-bromopyrazol-1-yl)borato-κ3 N,N′,N′′)-tris(tetrahydrofuran-κO)divanadium(II) – tetrahydrofuran (1/1), C34H57BBr6N6O4V2
Bonitatibus, Peter J.; Armstrong, William H.; Reiss, Guido J.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1101–1103; doi:10.1515/ncrs-2020-0187

data_8105390
_publ_section_title
;
 Preparation and crystal structure of a non-symmetrical vanadium(II)
 dimer:
 tri-\m2-bromido-(hydrogen-tris(3-isopropyl-4-bromopyrazol-1-yl)borato-\k3
 N,N&#x2032;,N&#x2032;&#x2032;)-tris(tetrahydrofuran-\kO)divanadium(II) --
 tetrahydrofuran (1/1), C34H57BBr6N6O4V2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1101
_journal_page_last               1103
_journal_paper_doi               10.1515/ncrs-2020-0187
_journal_volume                  235
_journal_year                    2020
_chemical_formula_sum            'C34 H57 B Br6 N6 O4 V2'
_chemical_formula_weight         1206.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.198(2)
_cell_length_b                   12.9497(11)
_cell_length_c                   20.496(2)
_cell_measurement_reflns_used    7646
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.56
_cell_measurement_theta_min      3.72
_cell_volume                     4564.6(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  SMART
_diffrn_measurement_method       omega
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1047
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26077
_diffrn_reflns_point_group_measured_fraction_full 0.710
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_theta_full        26.999
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.860
_exptl_absorpt_coefficient_mu    5.703
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_coef       0.00041(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7061
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0534P)^2^+6.3303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.381
_reflns_Friedel_fraction_full    0.403
_reflns_Friedel_fraction_max     0.403
_reflns_number_gt                6504
_reflns_number_total             7061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0187_suppl.cif
_cod_data_source_block           neu
_cod_original_cell_volume        4564.8(9)
_cod_database_code               8105390
_shelx_shelxl_version_number     2018/3