Crystal structure of (Z)-6-(dimethylamino)-3,3-bis(4-(dimethylamino)phenyl)-2-(2-(quinoxalin-2-ylmethylene)hydrazinyl)-2,3-dihydroinden-1-one, C35H35N7O
Zeng, Dai; Xing, Ai-Ping; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1023–1025; doi:10.1515/ncrs-2019-0238

data_8105925
_publ_section_title
;
 Crystal structure of
 (Z)-6-(dimethylamino)-3,3-bis(4-(dimethylamino)phenyl)-2-(2-(quinoxalin-2-ylmethylene)hydrazinyl)-2,3-dihydroinden-1-one,
 C35H35N7O
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1023
_journal_page_last               1025
_journal_paper_doi               10.1515/ncrs-2019-0238
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C35 H35 N7 O'
_chemical_formula_sum            'C35 H35 N7 O'
_chemical_formula_weight         569.70
_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                109.210(3)
_cell_angle_beta                 96.833(3)
_cell_angle_gamma                107.594(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2870(3)
_cell_length_b                   11.9918(4)
_cell_length_c                   13.8995(5)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      71.2700
_cell_measurement_theta_min      4.6260
_cell_volume                     1497.29(10)
_computing_cell_refinement       'CrysAlis^Pro^ [1] 2018)'
_computing_data_collection       'CrysAlis^Pro^ [1] 2018)'
_computing_data_reduction        'CrysAlis^Pro^ [1] 2018)'
_computing_molecular_graphics    'Olex2 [2]'
_computing_publication_material  'Olex2 [2]'
_computing_structure_refinement  'ShelXL-2015 [3]'
_computing_structure_solution    'ShelXT-2015 [4]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -113.00 -24.00   1.00    1.00    --  -40.81 -57.00  30.00   89
  2  \w    -90.00 -51.00   1.00    1.00    --  -40.81 -38.00-180.00   39
  3  \w    -90.00  -2.00   1.00    1.00    --  -40.81 125.00-120.00   88
  4  \w    -63.00  33.00   1.00    1.00    --  -40.81  38.00-180.00   96
  5  \w     34.00  59.00   1.00    1.00    --   40.81 -99.00-180.00   25
  6  \w     35.00 128.00   1.00    3.00    --  100.91 -61.00 -60.00   93
  7  \w     40.00 117.00   1.00    3.00    --  100.91-125.00 -90.00   77
  8  \w    114.00 167.00   1.00    3.00    --  100.91 125.00  60.00   53
  9  \w     91.00 117.00   1.00    3.00    --  100.91-125.00  30.00   26
 10  \w     72.00 130.00   1.00    3.00    --  100.91  61.00 -90.00   58
 11  \w     30.00  79.00   1.00    3.00    --  100.91 -30.00 120.00   49
 12  \w     56.00 117.00   1.00    3.00    --  100.91 -30.00  30.00   61
 13  \w     95.00 130.00   1.00    3.00    --  100.91 125.00-150.00   35
 14  \w     91.00 116.00   1.00    3.00    --  100.91-125.00 120.00   25
 15  \w    116.00 163.00   1.00    3.00    --  100.91  45.00 120.00   47
 16  \w     78.00 173.00   1.00    3.00    --  100.91  30.00  30.00   95
 17  \w     27.00 132.00   1.00    3.00    --  100.91 -77.00  60.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0549071000
_diffrn_orient_matrix_UB_12      -0.0991557000
_diffrn_orient_matrix_UB_13      -0.1136311000
_diffrn_orient_matrix_UB_21      0.0290187000
_diffrn_orient_matrix_UB_22      0.1072591000
_diffrn_orient_matrix_UB_23      -0.0414996000
_diffrn_orient_matrix_UB_31      0.1495653000
_diffrn_orient_matrix_UB_32      0.0003795000
_diffrn_orient_matrix_UB_33      -0.0018752000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10105
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.546
_diffrn_reflns_theta_min         3.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       cube
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0537P)^2^+0.3971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4888
_reflns_number_total             5642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0238_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1497.32(9)
_cod_database_code               8105925
_chemical_oxdiff_formula         'C H N O Cl Fe '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C12(H12), C16(H16), C17(H17),
 C21(H21), C22(H22), C26(H26), C27(H27), C29(H29), C30(H30), C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              24617
_shelx_hkl_checksum              42511
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.788