Crystal structure of (E)-3′,6′-bis(ethylamino)-2′,7′-dimethyl-2-((pyridin-2-ylmethylene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C32H31N5O2
Yuan, Juan; Cheng, Di; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 149–151; doi:10.1515/ncrs-2018-0239

data_8105571
_publ_section_title
;
 Crystal structure of
 (E)-3&#x2032;,6&#x2032;-bis(ethylamino)-2&#x2032;,7&#x2032;-dimethyl-2-((pyridin-2-ylmethylene)amino)spiro[isoindoline-1,9&#x2032;-xanthen]-3-one,
 C32H31N5O2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              149
_journal_page_last               151
_journal_paper_doi               10.1515/ncrs-2018-0239
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C32 H31 N5 O2'
_chemical_formula_sum            'C32 H31 N5 O2'
_chemical_formula_weight         517.62
_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                90.693(4)
_cell_angle_beta                 109.858(4)
_cell_angle_gamma                95.382(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9226(4)
_cell_length_b                   11.1446(7)
_cell_length_c                   12.6719(6)
_cell_measurement_reflns_used    5142
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.6430
_cell_measurement_theta_min      4.0040
_cell_volume                     1310.72(12)
_computing_cell_refinement       'CrysAlis^Pro^ [10]'
_computing_data_collection       'CrysAlis^Pro^ [10]'
_computing_data_reduction        'CrysAlis^Pro^ [10]'
_computing_molecular_graphics    'Olex2 [1]'
_computing_publication_material  'Olex2 [1]'
_computing_structure_refinement  'ShelXL-2015 [11]'
_computing_structure_solution    'ShelXS-2008 [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -58.00  27.00   1.00    1.00    --  -40.81  57.00 -30.00   85
  2  \w    -31.00  -2.00   1.00    1.00    --  -40.81 125.00   0.00   29
  3  \w   -115.00 -20.00   1.00    1.00    --  -40.81 -38.00  60.00   95
  4  \w      5.00  37.00   1.00    1.00    --   40.81 -99.00  30.00   32
  5  \w     40.00  96.00   1.00    1.00    --   40.81-125.00 120.00   56
  6  \w     39.00 109.00   1.00    3.00    --  112.00-125.00  60.00   70
  7  \w     73.00 100.00   1.00    3.00    --  112.00 -95.00  30.00   27
  8  \w     43.00 138.00   1.00    3.00    --  112.00 -45.00  90.00   95
  9  \w     59.00 163.00   1.00    3.00    --  112.00  15.00 -30.00  104
 10  \w    109.00 178.00   1.00    3.00    --  112.00  45.00-180.00   69
 11  \w     56.00  83.00   1.00    3.00    --  112.00 -95.00-180.00   27
 12  \w     41.00 114.00   1.00    3.00    --  112.00 -61.00-120.00   73
 13  \w     57.00 119.00   1.00    3.00    --  112.00-125.00 -90.00   62
 14  \w     37.00 118.00   1.00    3.00    --  112.00 -30.00   0.00   81
 15  \w     41.00 107.00   1.00    3.00    --  112.00 -95.00  90.00   66
 16  \w     30.00  58.00   1.00    3.00    --  112.00 -95.00   0.00   28
 17  \w     36.00  72.00   1.00    3.00    --  112.00 -30.00-180.00   36
 18  \w   -114.00 -87.00   1.00    1.00    --  -40.81-150.00  64.00   27
 19  \w   -113.00 -13.00   1.00    1.00    --  -40.81 -57.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0262482000
_diffrn_orient_matrix_UB_12      -0.1377957000
_diffrn_orient_matrix_UB_13      0.0060349000
_diffrn_orient_matrix_UB_21      0.0724521000
_diffrn_orient_matrix_UB_22      0.0116812000
_diffrn_orient_matrix_UB_23      0.1286719000
_diffrn_orient_matrix_UB_31      -0.1470008000
_diffrn_orient_matrix_UB_32      0.0140243000
_diffrn_orient_matrix_UB_33      0.0123221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.752
_diffrn_reflns_theta_min         3.713
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0804P)^2^+0.3458P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4778
_reflns_number_total             5295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0239_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105571
_chemical_oxdiff_formula         CHONCl
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99