Pnictogen-based vanadacyclobutadiene complexes.
Jafari, Mehrafshan G.; Russell, John B.; Myung, Hwan; Kwon, Seongyeon; Carroll, Patrick J.; Gau, Michael R.; Baik, Mu-Hyun; Mindiola, Daniel J.; Chemical science 15 (2024) 19752–19763; doi:10.1039/d4sc05884d

data_1572996
_publ_section_title
;
 Pnictogen-based vanadacyclobutadiene complexes.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              19752
_journal_page_last               19763
_journal_paper_doi               10.1039/d4sc05884d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C45 H64 N2 P V'
_chemical_formula_sum            'C45 H64 N2 P V'
_chemical_formula_weight         714.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-24
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r6015)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.771(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.668(3)
_cell_length_b                   10.2592(10)
_cell_length_c                   20.923(2)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.27
_cell_volume                     8081.7(13)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         1.948
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plank
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0639P)^2^+11.9316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                7093
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05884d2.cif
_cod_data_source_block           9404_complex3
_cod_depositor_comments
'Adding full bibliography for 1572995--1572996.cif.'
_cod_database_code               1572996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.951
_shelx_res_checksum              13742
_shelx_hkl_checksum              93778
_olex2_submission_special_instructions 'No special instructions were received'