Mechanochemical Production of Halogen-Bonded Solids Featuring P═O···I–C Motifs and Characterization via X-ray Diffraction, Solid-State Multinuclear Magnetic Resonance, and Density Functional Theory
Xu, Yijue; Viger-Gravel, Jasmine; Korobkov, Ilia; Bryce, David L.; The Journal of Physical Chemistry C 119 (2015) 27104–; doi:10.1021/acs.jpcc.5b09737

data_1554062
_publ_section_title
;
 Mechanochemical Production of Halogen-Bonded Solids Featuring
 P&#x2550;O&#x00B7;&#x00B7;&#x00B7;I--C Motifs and Characterization via
 X-ray Diffraction, Solid-State Multinuclear Magnetic Resonance, and
 Density Functional Theory
;
_journal_issue                   48
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              27104
_journal_paper_doi               10.1021/acs.jpcc.5b09737
_journal_volume                  119
_journal_year                    2015
_chemical_formula_sum            'C24 H15 F3 I3 O P'
_chemical_formula_weight         788.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                113.1738(10)
_cell_angle_beta                 96.9048(10)
_cell_angle_gamma                107.4200(11)
_cell_formula_units_Z            2
_cell_length_a                   9.7436(2)
_cell_length_b                   10.7585(2)
_cell_length_c                   13.5453(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.51
_cell_volume                     1198.74(5)
_computing_cell_refinement       'APEX II, Bruker (2012)'
_computing_data_collection       'APEX II, Bruker (2012)'
_computing_data_reduction        'XPREP, Bruker (2012)'
_computing_molecular_graphics    'SHELXTL, Bruker (2015)'
_computing_publication_material  'SHELXTL, Bruker (2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13769
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.382
_diffrn_reflns_theta_min         1.699
_exptl_absorpt_coefficient_mu    4.016
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0096(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.6169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5484
_reflns_number_total             5836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp5b09737_si_003.cif
_cod_data_source_block           db135
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'n/a' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        1198.74(4)
_cod_database_code               1554062
_shelx_estimated_absorpt_t_min   0.472
_shelx_estimated_absorpt_t_max   0.566
_shelxl_version_number           2013-4
_shelx_res_checksum              42033
_shelx_hkl_checksum              90265