Controlled assembly of a bicyclic porphyrinoid and its 3-dimensional boron difluoride arrays
Zhou, Weinan; Sarma, Tridib; Yang, Liu; Lei, Chuanhu; Sessler, Jonathan L.; Chemical Science 13 (2022) 7276–7282; doi:10.1039/D2SC01635D

data_1567078
_publ_section_title
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 Controlled assembly of a bicyclic porphyrinoid and its 3-dimensional
 boron difluoride arrays
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              7276
_journal_page_last               7282
_journal_paper_doi               10.1039/D2SC01635D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         '2(C H2 Cl2), C104 H105 B2 F4 N11, 5(C H4 O)'
_chemical_formula_sum            'C111 H129 B2 Cl4 F4 N11 O5'
_chemical_formula_weight         1936.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-02-08 deposited with the CCDC.	2022-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.9356(10)
_cell_length_b                   18.8132(4)
_cell_length_c                   29.4619(7)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      68.12
_cell_measurement_theta_min      3.00
_cell_volume                     21580.9(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            234927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.418
_diffrn_reflns_theta_min         2.269
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1144 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.7760.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       needle
_exptl_crystal_F_000             8208
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         19806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.1029
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3092
_refine_ls_wR_factor_ref         0.3439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13583
_reflns_number_total             19806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01635d2.cif
_cod_data_source_block           ta_a_sq
_cod_depositor_comments
'Adding full bibliography for 1567076--1567079.cif.'
_cod_database_code               1567078
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 O3(H3A)
2.b Riding coordinates and stretchable bonds:
 O2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C105(H10W,H10X), C111(H11D,H11E), C5(H5A,H5B), C7(H7A,H7B), C14(H14A,H14B),
 C16(H16A,H16B), C34(H34A,H34B), C36(H36A,H36B), C43(H43A,H43B), C45(H45A,H45B),
  C52(H52A,H52B), C54(H54A,H54B), C72(H72A,H72B), C74(H74A,H74B), C92(H92A,
 H92B), C94(H94A,H94B), C101(H10A,H10B), C103(H10F,H10G)
2.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), N8(H8), N10(H10), N11(H11), C19(H19), C20(H20), C23(H23),
 C24(H24), C26(H26), C29(H29), C38(H38), C57(H57), C58(H58), C61(H61), C62(H62),
  C64(H64), C67(H67), C77(H77), C78(H78), C81(H81), C82(H82), C84(H84),
 C87(H87), C96(H96)
2.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C73(H73A,H73B,H73C), C75(H75A,
 H75B,H75C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C102(H10C,H10D,H10E),
 C104(H10H,H10I,H10J), C106(H10K,H10L,H10M), C107(H10N,H10O,H10P), C108(H10Q,
 H10R,H10S), C109(H10T,H10U,H10V), C110(H11A,H11B,H11C)
2.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4), O5(H5C)
;
_shelx_res_checksum              72148
_shelx_fab_checksum              49440
_olex2_submission_special_instructions 'No special instructions were received'