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_7131216
_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         'C55 H69 K N2'
_chemical_formula_sum            'C55 H69 K N2'
_chemical_formula_weight         797.22
_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     dual
_audit_creation_date             2021-12-27
_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
_cell_angle_beta                 104.975(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0581(15)
_cell_length_b                   19.545(2)
_cell_length_c                   18.7522(17)
_cell_measurement_reflns_used    8229
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      44.95
_cell_measurement_theta_min      2.83
_cell_volume                     4977.5(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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      120.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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  0.1342
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42156
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.851
_diffrn_reflns_theta_min         2.831
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       stick
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1260P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4691
_reflns_number_total             9133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05736k2.cif
_cod_data_source_block           DPMK
_cod_depositor_comments
'Adding full bibliography for 7131216--7131219.cif.'
_cod_original_cell_volume        4977.4(9)
_cod_database_code               7131216
_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:
 C29(H29), C31(H31), C28(H28), C33(H33), C32(H32), C30(H30)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C24(H24), C8(H8), C26(H26), C19(H19), C21(H21), C2(H2), C3(H3),
 C12(H12), C14(H14), C51(H51), C49(H49), C48(H48), C46(H46), C50(H50)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C36(H36A,H36B,H36C), C53(H53A,H53B,
 H53C), C52(H52A,H52B,H52C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C43(H43A,
 H43B,H43C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C34(H34A,H34B,H34C),
 C55(H55A,H55B,H55C), C39(H39A,H39B,H39C), C54(H54A,H54B,H54C), C45(H45A,H45B,
 H45C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              5153
_shelx_hkl_checksum              4859
_olex2_submission_special_instructions 'No special instructions were received'