Solvent-Dependent Crystallization of 1-Hydro-6-carbaphosphatrane and Its Tautomer
Shin-ya Nakafuji; Junji Kobayashi; Takayuki Kawashima; Michael W. Schmidt; Inorganic Chemistry 44 (2005) 6500–6502; doi:10.1021/ic050679d

data_4309593
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science, 
The University of Tokyo
7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan
;
_publ_contact_author_email       takayuki@chem.s.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5800-6899
_publ_contact_author_name        'Takayuki Kawashima'
_publ_contact_author_phone       +81-3-5841-4338
_publ_section_title
;
Solvent-Dependent Crystallization of 1-Hydro-6-carbaphosphatrane and Its
Tautomer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6500
_journal_page_last               6502
_journal_paper_doi               10.1021/ic050679d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C34 H43 O3 P'
_chemical_formula_sum            'C34 H43 O3 P'
_chemical_formula_weight         530.65
_chemical_name_common            phosphonite
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(7)
_cell_angle_beta                 90.617(7)
_cell_angle_gamma                90.000(7)
_cell_formula_units_Z            4
_cell_length_a                   11.740(16)
_cell_length_b                   10.492(14)
_cell_length_c                   23.80(3)
_cell_measurement_temperature    120(2)
_cell_volume                     2931(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.756
_diffrn_measured_fraction_theta_max 0.756
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.1255
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12485
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.9752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0882
_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^)+(0.0391P)^2^+7.8028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                2402
_reflns_number_total             3897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050679dsi20050502_013609_2.cif
_cod_data_source_block           phosphonite
_cod_original_cell_volume        2932(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4309593