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_7715258
_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         'C184 H172 Na0.74 O48 V8, 3.75(C2 H3 N)'
_chemical_formula_sum            'C191.5 H183.25 N3.75 Na0.74 O48 V8'
_chemical_formula_weight         3729.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2024-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.623(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5339(3)
_cell_length_b                   36.8417(6)
_cell_length_c                   25.4428(4)
_cell_measurement_reflns_used    58436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.23
_cell_measurement_theta_min      3.23
_cell_volume                     19128.1(6)
_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-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0869
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            175601
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.165
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    3.794
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.540
_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            brown
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7739
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2578
_refine_ls_number_reflns         34845
_refine_ls_number_restraints     3520
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1059
_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^)+(0.1796P)^2^+53.5923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23854
_reflns_number_total             34845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00078a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715254--7715261.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C191.50 H183.25 N3.75 Na0.74 O48 V8'
_cod_database_code               7715258
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.286
_shelx_estimated_absorpt_t_max   0.863
_shelx_res_checksum              16201