Chemical Detection of Hydrogen Fluoride by the Phosphorus Congener of Cyclobutane-1,3-diyl.
Ueta, Yasuhiro; Mikami, Koichi; Ito, Shigekazu; Inorganic chemistry 54 (2015) 8778–8785; doi:10.1021/acs.inorgchem.5b01399

data_4346399
_publ_section_title
;
 Chemical Detection of Hydrogen Fluoride by the Phosphorus Congener of
 Cyclobutane-1,3-diyl.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8778
_journal_page_last               8785
_journal_paper_doi               10.1021/acs.inorgchem.5b01399
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C50 H78 Cl F2 N3 P2'
_chemical_formula_weight         856.54
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.3436(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7574(5)
_cell_length_b                   18.9788(7)
_cell_length_c                   18.1041(6)
_cell_measurement_temperature    123(2)
_cell_volume                     4933.7(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.400
_diffrn_reflns_theta_min         3.004
_exptl_absorpt_coefficient_mu    0.185
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         11156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9178
_reflns_number_total             11156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01399_si_002.cif
_cod_data_source_block           ueta012
_cod_original_sg_symbol_Hall     -P2yab
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4346399
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              29230
_shelx_hkl_checksum              12398