Analysis of the solvent effects on the crystal growth of peripherally chlorinated boron subphthalocyanines
Wojtkiewicz, Kacper; Lough, Alan; Bender, Timothy P.; CrystEngComm 24 (2022) 2791–2807; doi:10.1039/D1CE01320C

data_7244409
_publ_section_title
;
 Analysis of the solvent effects on the crystal growth of peripherally
 chlorinated boron subphthalocyanines
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2791
_journal_page_last               2807
_journal_paper_doi               10.1039/D1CE01320C
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety
'C30 H11 B Cl6 N6 O, 0.295(C6 H5 Cl), 0.705(C7 H16)'
_chemical_formula_sum            'C36.71 H23.76 B Cl6.3 N6 O'
_chemical_formula_weight         798.80
_chemical_name_systematic        PhO-Cl6BsubPc
_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     diff
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5724(6)
_cell_length_b                   20.9451(10)
_cell_length_c                   14.5210(8)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.65
_cell_volume                     3448.8(3)
_computing_cell_refinement       APEX3
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51213
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         1.796
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chlorobenzene/heptane'
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7945
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0669P)^2^+5.0142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4986
_reflns_number_total             7945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01320c2.cif
_cod_data_source_block           d19160_a
_cod_depositor_comments
'Adding full bibliography for 7244397--7244412.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36.71 H23.76 B Cl6.30 N6 O'
_cod_database_code               7244409
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              11638
_shelx_hkl_checksum              77835