Polymorphic form of 1,3,5-tris[(diphenylphosphine oxide)methyl]benzene acetonitrile solvate monohydrate
Kruszynski, Rafal; Wieczorek, Wanda; Acta Crystallographica Section E 57 (2001) o624–o626; doi:10.1107/S1600536801010157

data_2200462
_publ_section_title
;
 Polymorphic form of 1,3,5-tris[(diphenylphosphine oxide)methyl]benzene
 acetonitrile solvate monohydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o624
_journal_page_last               o626
_journal_paper_doi               10.1107/S1600536801010157
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C45 H39 O3 P3, C2 H3 N, H2 O'
_chemical_formula_moiety         'C45 H39 O3 P3, C2 H3 N, H2 O'
_chemical_formula_sum            'C47 H44 N O4 P3'
_chemical_formula_weight         779.74
_chemical_name_systematic
;
benzene-1,3,5-triyltrismethylenetris(diphenylphosphine oxide) acetonitrile
solvate monohydrate
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.034(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.3382(14)
_cell_length_b                   8.6418(9)
_cell_length_c                   15.9748(11)
_cell_measurement_reflns_used    8473
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     2045.0(3)
_computing_cell_refinement       'CrysAlis RED (UNIL IC & Kuma, 2000)'
_computing_data_collection       'CrysAlis CCD (UNIL IC & Kuma, 2000)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
'XP in SHELXTL/PC (Sheldrick, 1990b) and ORTEP-3 (Farrugia 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_measured_fraction_theta_full .990
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  'Kuma KM4-CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0602
_diffrn_reflns_av_sigmaI/netI    .0350
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20214
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.54
_diffrn_standards_decay_%        -1.12
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .190
_exptl_absorpt_correction_T_max  .9277
_exptl_absorpt_correction_T_min  .8943
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1999)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             820
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .40
_refine_diff_density_max         .290
_refine_diff_density_min         -.416
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .24(15)
_refine_ls_extinction_coef       .0083(5)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6643
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          .0794
_refine_ls_R_factor_gt           .0785
_refine_ls_shift/su_max          .003
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0113P)^2^+5.8292P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1640
_reflns_number_gt                6532
_reflns_number_total             6643
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6030.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-24

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2200462
_cod_database_fobs_code          2200462