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_4309592
_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            6-carbaphosphatrane
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.8927(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.220(4)
_cell_length_b                   11.916(3)
_cell_length_c                   17.379(4)
_cell_measurement_temperature    120(2)
_cell_volume                     3059.7(13)
_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 0.649
_diffrn_measured_fraction_theta_max 0.649
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15222
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9704
_exptl_absorpt_correction_T_min  0.9476
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0886P)^2^+2.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                3981
_reflns_number_total             4563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050679dsi20050502_013609_1.cif
_cod_data_source_block           6-carbaphosphatrane
_cod_original_cell_volume        3059.6(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4309592