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_7244412
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H10 B Cl6 I N6 O'
_chemical_formula_sum            'C30 H10 B Cl6 I N6 O'
_chemical_formula_weight         820.85
_chemical_name_systematic        IPhO-Cl6BsubPc
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8915(6)
_cell_length_b                   15.1172(6)
_cell_length_c                   23.9514(9)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.52
_cell_volume                     5754.0(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0491
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            143954
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         1.859
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_description       Shard
_exptl_crystal_F_000             3200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichlorobenzene/dimethoxybezene/heptane'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
; 
 Flack x determined using 5602 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         13197
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0437P)^2^+4.7539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12219
_reflns_number_total             13197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01320c2.cif
_cod_data_source_block           d2017a_a
_cod_depositor_comments
'Adding full bibliography for 7244397--7244412.cif.'
_cod_database_code               7244412
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.602
_shelx_estimated_absorpt_t_max   0.674
_shelx_res_checksum              56560
_shelx_hkl_checksum              31041