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_4345779
_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         '4(C20 H35 N P3), C4 H10 O, 4(C F3 O3 S)'
_chemical_formula_sum            'C88 H150 F12 N4 O13 P12 S4'
_chemical_formula_weight         2199.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.470(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   51.906(3)
_cell_length_b                   11.3247(6)
_cell_length_c                   20.0014(13)
_cell_measurement_reflns_used    6886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.26
_cell_volume                     11214.9(12)
_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 0.997
_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  0.1136
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            89361
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.823
_diffrn_reflns_theta_min         0.822
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8389.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11997
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+33.4576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8204
_reflns_number_total             11997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00086_si_002.cif
_cod_data_source_block           5Ph
_cod_database_code               4345779
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-F4 \\sim C42A-F4A \\sim C42-F5 \\sim C42A-F5A \\sim C42-F6 \\sim C42A-F6A
 with sigma of 0.02
 C42-S2 \\sim C42A-S2A
 with sigma of 0.02
 S2-O4 \\sim S2A-O4A \\sim S2-O5 \\sim S2A-O5A \\sim S2-O6 \\sim S2A-O6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5A) = Uanis(F5)
Uanis(F6) = Uanis(F6A)
Uanis(F4A) = Uanis(F4)
Uanis(C42A) = Uanis(C42)
Uanis(O5) = Uanis(O5A)
Uanis(O4) = Uanis(O4A)
Uanis(S2) = Uanis(S2A)
Uanis(O6A) = Uanis(O6)
4. Others
 Fixed Sof: O7(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5)
 S2A(0.61254) F4A(0.61254) F5A(0.61254) F6A(0.61254) O4A(0.61254) O5A(0.61254)
 O6A(0.61254) C42A(0.61254) S2(0.38746) F4(0.38746) F5(0.38746) F6(0.38746)
 O4(0.38746) O5(0.38746) O6(0.38746) C42(0.38746)
5.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C23(H23), C24(H24), C25(H25),
 C26(H26), C27(H27)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              2189
_shelx_hkl_checksum              89058
_olex2_submission_special_instructions 'No special instructions were received'