Crystal structure of 3-[(triisopropylsilanyl)-ethynyl]-6a,12a-dihydro-1H-1,4-diaza-benzo[α]anthracene-2,7,12-trione, C27H28N2O3Si
Zhu, Lei; Luo, Na; Chen, Jinyang; Zhang, Mingzhong; Zhao, Jingzhe; Miao, Shaobin; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1129–1131; doi:10.1515/ncrs-2020-0200

data_8105398
_publ_section_title
;
 Crystal structure of
 3-[(triisopropylsilanyl)-ethynyl]-6a,12a-dihydro-1H-1,4-diaza-benzo[\a]anthracene-2,7,12-trione,
 C27H28N2O3Si
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1129
_journal_page_last               1131
_journal_paper_doi               10.1515/ncrs-2020-0200
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C27 H28 N2 O3 Si'
_chemical_formula_sum            'C27 H28 N2 O3 Si'
_chemical_formula_weight         456.60
_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
_cell_angle_alpha                97.002(5)
_cell_angle_beta                 98.703(5)
_cell_angle_gamma                95.739(5)
_cell_formula_units_Z            2
_cell_length_a                   7.5098(4)
_cell_length_b                   7.8881(4)
_cell_length_c                   20.8904(14)
_cell_measurement_reflns_used    2224
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.9400
_cell_measurement_theta_min      3.6680
_cell_volume                     1205.25(12)
_computing_cell_refinement       'Bruker APEX2 [1])'
_computing_data_collection       'Bruker APEX2 [1])'
_computing_data_reduction        'Bruker APEX2 [1])'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009[3])'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009[3])'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015[2])'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7540
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         3.507
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.8213
_exptl_absorpt_correction_T_min  0.0123
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.5457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2823
_reflns_number_total             4243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0200_suppl.cif
_cod_data_source_block           ww
_cod_database_code               8105398
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C26, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C19(H19), C23(H23), C26(H26)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;