The crystal structure of 10-(3,5-di(pyridin-4-yl)phenyl)-10H-phenoxazine dihydrate, C28H23N3O3
Yang, Zhuqing; Hou, Meng; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 605–607; doi:10.1515/ncrs-2021-0001

data_8104779
_publ_section_title
;
 The crystal structure of 10-(3,5-di(pyridin-4-yl)phenyl)-10H-phenoxazine
 dihydrate, C28H23N3O3
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              605
_journal_page_last               607
_journal_paper_doi               10.1515/ncrs-2021-0001
_journal_volume                  236
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H19 N3 O, 2(H2 O)'
_chemical_formula_sum            'C28 H23 N3 O3'
_chemical_formula_weight         449.49
_chemical_name_systematic
;
10-(3,5-di(pyridin-4-yl)phenyl)-10H-phenoxazine
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0466(11)
_cell_length_b                   5.2448(3)
_cell_length_c                   14.4825(7)
_cell_measurement_reflns_used    1726
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1030
_cell_measurement_theta_min      3.0050
_cell_volume                     2206.32(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f [1]'
_computing_data_collection       'CrysAlisPro 1.171.38.43f [1]'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f [1]'
_computing_molecular_graphics    'Olex2 1.3 [2]'
_computing_publication_material  'Olex2 1.3 [2]'
_computing_structure_refinement  'SHELXL 2018/3 [3]'
_computing_structure_solution    'SHELXT 2018/3 [3]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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    -41.00  20.00   1.00    3.23    --  -40.98   0.00-150.00   61
  2  \w     16.00  96.00   1.00    3.23    --   40.98  38.00-150.00   80
  3  \w     81.00 178.00   1.00    5.00    --  106.95  45.00   0.00   97
  4  \w     55.00  89.00   1.00    5.00    --  106.95 -94.00 150.00   34
  5  \w     25.00  52.00   1.00    5.00    --  106.95 -94.00 150.00   27
  6  \w     36.00 138.00   1.00    5.00    --  106.95 -77.00-150.00  102
  7  \w   -106.00 -71.00   1.00    3.23    --  -40.98   0.00-150.00   35
;
_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      -0.0346229000
_diffrn_orient_matrix_UB_12      0.0752970000
_diffrn_orient_matrix_UB_13      -0.0792040000
_diffrn_orient_matrix_UB_21      -0.0400375000
_diffrn_orient_matrix_UB_22      -0.0615023000
_diffrn_orient_matrix_UB_23      0.0906522000
_diffrn_orient_matrix_UB_31      0.0033203000
_diffrn_orient_matrix_UB_32      0.0431327000
_diffrn_orient_matrix_UB_33      0.2679837000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5115
_diffrn_reflns_point_group_measured_fraction_full 0.813
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.605
_diffrn_reflns_theta_min         3.043
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83206
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 920 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         3451
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.526
_reflns_Friedel_fraction_full    0.609
_reflns_Friedel_fraction_max     0.556
_reflns_number_gt                3078
_reflns_number_total             3451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0001_suppl.cif
_cod_data_source_block           136-2
_cod_database_code               8104779
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28)
;