A Room-Temperature-Stable Phosphanorcaradiene.
Liu, Liu Leo; Zhou, Jiliang; Andrews, Ryan; Stephan, Douglas W.; Journal of the American Chemical Society 140 (2018) 7466–7470; doi:10.1021/jacs.8b04930

data_4132576
_publ_section_title
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 A Room-Temperature-Stable Phosphanorcaradiene.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7466
_journal_page_last               7470
_journal_paper_doi               10.1021/jacs.8b04930
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C F3 O3 S, C18 H37 N2 Si, 0.5(C6 H5 Cl)'
_chemical_formula_sum            'C22 H39.5 Cl0.5 F3 N2 O3 S Si'
_chemical_formula_weight         514.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.018(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2238(6)
_cell_length_b                   17.2610(12)
_cell_length_c                   17.5861(11)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.36
_cell_volume                     2772.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0822 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8749.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0550P)^2^+1.1145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4143
_reflns_number_total             6613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04930_si_002.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C22 H39.50 Cl0.50 F3 N2 O3 S Si'
_cod_database_code               4132576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.951
_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. Others
 Fixed Sof: Cl1S(0.5) C1S(0.5) C2S(0.5) H2S(0.5) C3S(0.5) H3S(0.5) C4S(0.5)
 H4S(0.5) C5S(0.5) H5S(0.5) C6S(0.5) H6S(0.5)
3.a Ternary CH refined with riding coordinates:
 C00C(H00C), C00F(H00F), C00G(H00G), C00J(H00J)
3.b Aromatic/amide H refined with riding coordinates:
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
3.c Idealised Me refined as rotating group:
 C00I(H00A,H00B,H00D), C00K(H00E,H00H,H00I), C00M(H00K,H00L,H00M), C00N(H00N,
 H00O,H00P), C00O(H00Q,H00R,H00S), C00P(H00T,H00U,H00V), C00R(H00W,H00X,H00Y),
 C00S(H00Z,H,HA), C00T(H00,HB,HC), C00U(H0AA,HD,HE), C00V(H1AA,HF,HG)
;
_shelx_res_checksum              58903
_shelx_hkl_checksum              58371
_olex2_submission_special_instructions 'No special instructions were received'