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_7131219
_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 Cl2 N2 Sb, 2(C6 H6)'
_chemical_formula_sum            'C60 H73 Cl2 N2 Sb'
_chemical_formula_weight         1014.85
_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
;
2022-10-20 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.015(4)
_cell_angle_beta                 103.015(4)
_cell_angle_gamma                114.680(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7747(14)
_cell_length_b                   13.6594(16)
_cell_length_c                   20.446(2)
_cell_measurement_reflns_used    9448
_cell_measurement_temperature    129(2)
_cell_measurement_theta_max      54.11
_cell_measurement_theta_min      5.73
_cell_volume                     2894.7(6)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      129.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.957
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_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            48124
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.344
_diffrn_reflns_theta_min         1.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.274
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4637
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1299 before and 0.0801 after correction.
The Ratio of minimum to maximum transmission is 0.6178.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.048
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         10329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0358P)^2^+46.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10143
_reflns_number_total             10329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05736k2.cif
_cod_data_source_block           DPMSbCl2
_cod_depositor_comments
'Adding full bibliography for 7131216--7131219.cif.'
_cod_database_code               7131219
_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
2.a Ternary CH refined with riding coordinates:
 C48(H48), C25(H25), C27(H27), C40(H40), C26(H26), C44(H44)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C23(H23), C2(H2), C8(H8), C7(H7), C21(H21), C12(H12), C14(H14),
 C53(H53), C36(H36), C38(H38), C54(H54), C52(H52), C49(H49), C50(H50), C57(H57),
  C51(H51), C55(H55), C60(H60), C58(H58), C59(H59), C56(H56)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C), C46(H46A,H46B,
 H46C), C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C47(H47A,H47B,H47C), C31(H31A,
 H31B,H31C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              36406
_shelx_hkl_checksum              58801
_shelx_fab_checksum              6133
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'