Crystalline heaviest pnictogen-dipyrromethenes: isolation, characterization, and reactivity.
Liu, Chen; Dai, Yuyang; Han, Qiqi; Liu, Chunmeng; Su, Yuanting; Chemical communications (Cambridge, England) 59 (2023) 2161–2164; doi:10.1039/d2cc05736k

data_7131217
_publ_section_title
;
 Crystalline heaviest pnictogen-dipyrromethenes: isolation,
 characterization, and reactivity.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2161
_journal_page_last               2164
_journal_paper_doi               10.1039/d2cc05736k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C48 H61 Bi Cl2 N2, 2(C7 H8)'
_chemical_formula_sum            'C62 H77 Bi Cl2 N2'
_chemical_formula_weight         1130.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-22 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                89.7190(10)
_cell_angle_beta                 77.7200(10)
_cell_angle_gamma                65.4490(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8029(6)
_cell_length_b                   13.8511(7)
_cell_length_c                   20.2711(11)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      54.04
_cell_measurement_theta_min      2.63
_cell_volume                     2932.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26039
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.939
_diffrn_reflns_theta_min         1.949
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.840
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.781
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+4.1605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10283
_reflns_number_total             10388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05736k2.cif
_cod_data_source_block           DPMBiCl2
_cod_depositor_comments
'Adding full bibliography for 7131216--7131219.cif.'
_cod_database_code               7131217
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C46A-C37 \\sim C46-C37
 with sigma of 0.02
 C46-C47A \\sim C47A-C46A
 with sigma of 0.02
3. Others
 Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=1-FVAR(1)
 Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C40(H40), C26(H26), C41(H41), C27(H27), C46A(H46A), C46(H46)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C21(H21), C12(H12), C23(H23), C2(H2), C3(H3), C61(H61),
 C38(H38), C14(H14), C52(H52), C59(H59), C51(H51), C54(H54), C56(H56), C36(H36),
  C49(H49), C50(H50), C58(H58), C57(H57)
4.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C48(H48D,H48E,H48F), C48(H48A,H48B,
 H48C), C28(H28A,H28B,H28C), C45(H45A,H45B,H45C), C43(H43A,H43B,H43C), C32(H32A,
 H32B,H32C), C42(H42A,H42B,H42C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C31(H31A,H31B,H31C), C29(H29A,H29B,
 H29C), C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C47A(H47A,H47B,H47C),
 C47(H47D,H47E,H47F)
;
_shelx_res_checksum              97378
_shelx_hkl_checksum              19061
_shelx_fab_checksum              70852
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'