Crystal structure of 3,6-di-tert-butyl-1-iodo-9-methyl-8-(pyren-1-ylethynyl)-9H-carbazole, C39H34IN
Hu, Xin; Jia, Guo-Kai; Ding, Man-Hua; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 485–487; doi:10.1515/ncrs-2022-0094

data_8105730
_publ_section_title
;
 Crystal structure of
 3,6-di-tert-butyl-1-iodo-9-methyl-8-(pyren-1-ylethynyl)-9H-carbazole,
 C39H34IN
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              485
_journal_page_last               487
_journal_paper_doi               10.1515/ncrs-2022-0094
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C39 H34 I N'
_chemical_formula_sum            'C39 H34 I N'
_chemical_formula_weight         643.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.500(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.651(2)
_cell_length_b                   7.0023(14)
_cell_length_c                   18.716(4)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.33
_cell_measurement_theta_min      2.63
_cell_volume                     1513.9(5)
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.097
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            corlourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   1.00
_exptl_transmission_factor_min   0.98
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0483P)^2^+0.7287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2478
_reflns_number_total             3700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0094_suppl.cif
_cod_data_source_block           11
_cod_original_cell_volume        1513.8(5)
_cod_database_code               8105730
_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. Others
 Fixed Sof: H9B(0.5) H9C(0.5) H16B(0.5) H16C(0.5) H19B(0.5) H19C(0.5)
3.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C13(H13), C15(H15), C23(H23), C24(H24), C26(H26), C27(H27),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              27000
_shelx_hkl_checksum              82075
_olex2_submission_special_instructions 'No special instructions were received'