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_7715257
_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 Na0.45 O48 V8, 6.38(C2 H3 N)'
_chemical_formula_sum            'C204.77 H207.15 N6.38 Na0.45 O48 V8'
_chemical_formula_weight         3943.41
_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     iterative
_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                 111.1170(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.4100(2)
_cell_length_b                   19.24118(15)
_cell_length_c                   25.4130(3)
_cell_measurement_reflns_used    68244
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.85
_cell_measurement_theta_min      2.23
_cell_volume                     9765.95(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF equipped with Varimax confocal mirrors and 
an AFC11 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            171151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.743
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019). 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             4107
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.091
_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     1464
_refine_ls_number_reflns         17412
_refine_ls_number_restraints     1819
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1427P)^2^+9.3579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14474
_reflns_number_total             17412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00078a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7715254--7715261.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7715257
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.400
_shelx_estimated_absorpt_t_max   0.706
_shelx_res_checksum              4817
_shelx_fab_checksum              19285