An untethered C3v-symmetric triarylphosphine oxide locked by intermolecular hydrogen bonding
Carroll, Timothy G.; Hunt, Camden; Garwick, Rachel; Wu, Guang; Dobrovetsky, Roman; Ménard, Gabriel; Chemical Communications  (2019) –; doi:10.1039/C9CC01128E

data_7123130
_publ_section_title
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 An untethered C3v-symmetric triarylphosphine oxide locked by
 intermolecular hydrogen bonding
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01128E
_journal_year                    2019
_chemical_formula_moiety         '0.5(C102 H66 O14 P2 V6)'
_chemical_formula_sum            'C51 H33 O7 P V3'
_chemical_formula_weight         941.61
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_Hall           '-P 6c 2'
_space_group_name_H-M_alt        'P 63/m c m'
_symmetry_Int_Tables_number      193
_symmetry_space_group_name_Hall  '-P 6c 2'
_symmetry_space_group_name_H-M   'P 63/m c m'
_audit_creation_date             2018-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-02-06 deposited with the CCDC.    2019-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.033(2)
_cell_length_b                   15.033(2)
_cell_length_c                   11.491(3)
_cell_measurement_reflns_used    1373
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.47
_cell_measurement_theta_min      2.71
_cell_volume                     2248.9(7)
_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  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      109.87
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11757
_diffrn_reflns_theta_full        24.8402
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.8929.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.3905
_exptl_crystal_description       'blue plate'
_exptl_crystal_F_000             960.5080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.0794
_refine_diff_density_min         -2.2085
_refine_diff_density_rms         0.1956
_refine_ls_d_res_high            0.8459
_refine_ls_d_res_low             13.0186
_refine_ls_goodness_of_fit_ref   1.0511
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     61
_refine_ls_number_reflns         733
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.0380
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.1347
_refine_ls_shift/su_max          0.0025
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+49.7094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2394
_refine_ls_wR_factor_ref         0.2494
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                582
_reflns_number_total             733
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc01128e2.cif
_cod_data_source_block           tgc266_blue_0m_a
_cod_original_cell_volume        2248.8(7)
_cod_database_code               7123130
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H6-C6
 1 with sigma of 0.01
 C8-C9 \\sim C9-C10 \\sim C8B-C9B \\sim C9B-C10B
 with sigma of 0.01
 C0aa-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C0aa-C6 \\sim C5-C6
 with sigma of 0.01
 C0aa-C3 \\sim C2-C4 \\sim C3-C5 \\sim C5-C0aa
 with sigma of 0.01
 H6-C0aa \\sim H6-C5
 with sigma of 0.01
3. Restrained planarity
 C0aa, C2, C3, C4, C5, C6, H6
 with sigma of 0.1
4. Others
 Fixed Sof: C8(0.25) H8(0.25) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C8B(0.25)
 H8B(0.25) C9B(0.5) H9B(0.5) C10B(0.5) H10B(0.5) C0aa(0.25) C2(0.25) C3(0.25)
 C5(0.25) C6(0.25) H6(0.25) O2(0.25) O3(0.25) C1(0.25) P1(0.0833) O1(0.08333)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C8B(H8B), C9B(H9B), C10B(H10B)
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_olex2_submission_special_instructions 'No special instructions were received'