Ring size effects in cyclic fluorophosphites: ligands that span the bonding space between phosphites and PF3
Miles-Hobbs, Alexandra M.; Hunt, Eliza; Pringle, Paul. G.; Sparkes, Hazel A.; Dalton Transactions  (2019) –; doi:10.1039/C9DT00893D

data_7049666
_publ_section_title
;
 Ring size effects in cyclic fluorophosphites: ligands that span the
 bonding space between phosphites and PF3
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00893D
_journal_year                    2019
_chemical_formula_moiety         'C40 H24 F4 O8 P4 Pt, C6 H5 Cl'
_chemical_formula_sum            'C46 H29 Cl F4 O8 P4 Pt'
_chemical_formula_weight         1140.11
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-19 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2985(4)
_cell_length_b                   15.2985(4)
_cell_length_c                   8.8050(3)
_cell_measurement_reflns_used    2923
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      2.31
_cell_volume                     2060.76(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex suite'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.881
_diffrn_reflns_theta_min         1.883
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.701
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0995 before and 0.0610 after correction. The Ratio of minimum to maximum transmission is 0.7406. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2476
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1935
_reflns_number_total             2476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00893d2.cif
_cod_data_source_block           4b
_cod_original_cell_volume        2060.76(13)
_cod_database_code               7049666
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.334
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C12-Cl1 \\sim C16-Cl1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(Cl1) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl1(0.25) C11(0.25) C12(0.25) H12(0.25) C13(0.25) H13(0.25)
 C14(0.25) H14(0.25) C15(0.25) H15(0.25) C16(0.25) H16(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C3(H3), C8(H8), C10(H10), C4(H4), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16)
5.b Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16)
;
_shelx_res_checksum              95342
_olex2_submission_special_instructions 'No special instructions were received'