Tris(3-hydroxyimino-1-methylindolin-2-one) monohydrate
Miao, Yanqing; Zhang, Xiaoqing; Liu, Chunye; You, Jing; Acta Crystallographica Section E 67 (2011) o1291–; doi:10.1107/S1600536811015418

data_2230393
_publ_section_title
;
 Tris(3-hydroxyimino-1-methylindolin-2-one) monohydrate
;
_journal_coeditor_code           JJ2082
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1291
_journal_paper_doi               10.1107/S1600536811015418
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '3C9 H8 N2 O2, H2 O'
_chemical_formula_moiety         '3(C9 H8 N2 O2), H2 O'
_chemical_formula_sum            'C27 H26 N6 O7'
_chemical_formula_weight         546.54
_chemical_name_systematic
;
Tris(3-hydroxyimino-1-methylindolin-2-one) monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.335(3)
_cell_angle_beta                 101.013(3)
_cell_angle_gamma                112.784(3)
_cell_formula_units_Z            2
_cell_length_a                   8.920(3)
_cell_length_b                   10.811(4)
_cell_length_c                   14.915(5)
_cell_measurement_reflns_used    3022
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     1294.1(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7872
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.214
_refine_ls_extinction_coef       0.029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                3154
_reflns_number_total             4512
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2082.cif
_cod_data_source_block           I
_cod_original_cell_volume        1294.1(7)
_cod_database_code               2230393
_cod_database_fobs_code          2230393