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_4346398
_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            'C54 H87 Cl N4 P2'
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                97.5380(10)
_cell_angle_beta                 98.853(2)
_cell_angle_gamma                95.676(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4898(6)
_cell_length_b                   10.8011(5)
_cell_length_c                   26.3998(12)
_cell_measurement_temperature    123(2)
_cell_volume                     2631.0(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  RAXIS-Rapid
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25689
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    0.171
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         11937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.734
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.0954
_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          0.2373
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_reflns_number_gt                6477
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01399_si_004.cif
_cod_data_source_block           ueta009
_cod_database_code               4346398
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              38440
_shelx_hkl_checksum              20955