Synthesis, Crystal Structure, EPR, and DFT Studies of an Unusually Distorted Vanadium(II) Complex
Bonitatibus, Peter John; Alvarez, Santiago; Armstrong, William H.; Baldansuren, Amgalanbaatar; Gaspard, Mallory E.; Lakshmi, K. V.; Ziegler, Micah S.; Charles, Philip; Dalton Transactions  (2022) –; doi:10.1039/D2DT02392J

data_7710868
_publ_section_title
;
 Synthesis, Crystal Structure, EPR, and DFT Studies of an Unusually
 Distorted Vanadium(II) Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02392J
_journal_year                    2022
_chemical_formula_moiety         'C48 H64 O4 V'
_chemical_formula_sum            'C48 H64 O4 V'
_chemical_formula_weight         755.93
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-21 deposited with the CCDC.	2022-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1309(4)
_cell_length_b                   24.5283(9)
_cell_length_c                   18.0181(7)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      56.65
_cell_measurement_theta_min      3.75
_cell_volume                     4400.5(3)
_computing_cell_refinement       'SHELXTL V5.03 (Bruker, 1995)'
_computing_data_collection       'SMART V4.031 (Bruker, 1994)'
_computing_data_reduction        'SAINT V4.028 (Bruker, 1994-6)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'CCD rotation images, phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1340
_diffrn_reflns_av_unetI/netI     0.1260
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18169
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         2.020
_diffrn_source                   'Mo K/a fine-focus selaed tube'
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1628
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+7.3195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3975
_reflns_number_total             6259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02392j2.cif
_cod_data_source_block           end1
_cod_database_code               7710868
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C00M(H00M), C00R(H00R), C00Z(H00Z)
2.b Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00U(H00D,H00E,H00F), C00V(H00G,H00H,H00I), C00Y(H00J,
 H00K,H00L), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C013(H01G,H01H,H01I),
 C014(H01J,H01K,H01L), C015(H01M,H01N,H01O), C016(H01P,H01Q,H01R), C017(H01S,
 H01T,H01U), C018(H01V,H01W,H01X), C019(H01Y,H,HA), C01A(H01Z,HB,HC), C01C(H01,
 HD,HE), C01D(H0AA,HF,HG), C01E(H1AA,HH,HI), C01F(H2AA,HJ,HK), C01G(H3AA,HL,HM),
  C01H(H4AA,HN,HO)
;
_olex2_submission_special_instructions 'No special instructions were received'