Reaction of Ph<sub>2</sub>C(X)(CO<sub>2</sub>H) (X = OH, NH<sub>2</sub>) with [VO(OR)<sub>3</sub>] (R = Et, <i>n</i>Pr): structure, magnetic susceptibility and ROP capability.
Glenister, Mollie A.; Frese, Josef W. A.; Elsegood, Mark R. J.; Canaj, Angelos B.; Brechin, Euan K.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5351–5355; doi:10.1039/d4dt00078a

data_7715255
_publ_section_title
;
 Reaction of Ph<sub>2</sub>C(X)(CO<sub>2</sub>H) (X = OH, NH<sub>2</sub>)
 with [VO(OR)<sub>3</sub>] (R = Et, <i>n</i>Pr): structure, magnetic
 susceptibility and ROP capability.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5351
_journal_page_last               5355
_journal_paper_doi               10.1039/d4dt00078a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C192 H188 K0.20 O48 V8, 7(N C2 H3)'
_chemical_formula_sum            'C206 H209 K0.2 N7 O48 V8'
_chemical_formula_weight         3966.13
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2024-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.554(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.378(3)
_cell_length_b                   19.274(3)
_cell_length_c                   25.446(4)
_cell_measurement_reflns_used    10689
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.23
_cell_volume                     9752(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6943
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            94774
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.619
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.437
_diffrn_source                   'Daresbury SRS station 9.8'
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            'Dark purple'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Diamond block'
_exptl_crystal_F_000             4132
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         24018
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1437P)^2^+1.2873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14951
_reflns_number_total             24018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00078a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7715254--7715261.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C206 H209 K0.20 N7 O48 V8'
_cod_database_code               7715255
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              37285
_shelx_fab_checksum              25011