Influence of Ring Strain and Bond Polarization on the Ring Expansion of Phosphorus Homocycles.
Chitnis, Saurabh S.; Musgrave, Rebecca A.; Sparkes, Hazel A.; Pridmore, Natalie E.; Annibale, Vincent T.; Manners, Ian; Inorganic chemistry 56 (2017) 4522–4538; doi:10.1021/acs.inorgchem.7b00086

data_4345782
_publ_section_title
;
 Influence of Ring Strain and Bond Polarization on the Ring Expansion of
 Phosphorus Homocycles.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4522
_journal_page_last               4538
_journal_paper_doi               10.1021/acs.inorgchem.7b00086
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C11 H19 Cl N2 P, C F3 O3 S'
_chemical_formula_sum            'C12 H19 Cl F3 N2 O3 P S'
_chemical_formula_weight         394.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                81.310(2)
_cell_angle_beta                 85.249(3)
_cell_angle_gamma                73.965(2)
_cell_formula_units_Z            6
_cell_length_a                   12.8025(4)
_cell_length_b                   13.5213(4)
_cell_length_c                   16.1587(6)
_cell_measurement_reflns_used    3682
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.60
_cell_measurement_theta_min      2.18
_cell_volume                     2655.00(15)
_computing_data_collection       'Apex 3 (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_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  0.1011
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44440
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.180
_diffrn_reflns_theta_min         1.276
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0619 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.8879.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         11741
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1036P)^2^+2.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6172
_reflns_number_total             11741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00086_si_002.cif
_cod_data_source_block           12Cl
_cod_database_code               4345782
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-C34 = F2-C34 = F3-C34 = F1A-C34A = F2A-C34A = F3A-C34A
 1.33 with sigma of 0.01
 S1-C34 = S1AB-C34A
 1.81 with sigma of 0.01
 S1-O2 = S1AB-O1A = S1-O1 = S1AB-O2A = S1AB-O3A = S1-O3
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim F1 \\sim F2 \\sim F3 \\sim O1 \\sim O2 \\sim O3 \\sim C34 \\sim S1AB
\\sim F1A \\sim F2A \\sim F3A \\sim O1A \\sim O2A \\sim O3A \\sim C34A: within
2A with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: S1(0.67417) F1(0.67417) F2(0.67417) F3(0.67417) O1(0.67417)
 O2(0.67417) O3(0.67417) C34(0.67417) S1AB(0.32583) F1A(0.32583) F2A(0.32583)
 F3A(0.32583) O1A(0.32583) O2A(0.32583) O3A(0.32583) C34A(0.32583)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16),
 C23(H23), C24(H24), C26(H26), C27(H27)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              3549
_shelx_hkl_checksum              63292
_olex2_submission_special_instructions 'No special instructions were received'