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_7123132
_publ_section_title
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 An untethered C3v-symmetric triarylphosphine oxide locked by
 intermolecular hydrogen bonding
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01128E
_journal_year                    2019
_chemical_formula_moiety         'B C24 F20, C Cl2, C29 H24 O3 P V'
_chemical_formula_sum            'C54 H24 B Cl2 F20 O3 P V'
_chemical_formula_weight         1264.40
_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_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2019-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-06 deposited with the CCDC.    2019-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.089(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0426(19)
_cell_length_b                   33.159(2)
_cell_length_c                   16.5246(11)
_cell_measurement_reflns_used    7185
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.24
_cell_volume                     12427.2(15)
_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      100.12
_diffrn_measured_fraction_theta_full 0.9864
_diffrn_measured_fraction_theta_max 0.9864
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36579
_diffrn_reflns_theta_full        26.5205
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         1.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0550 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.8982.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.3515
_exptl_crystal_description       'red plate'
_exptl_crystal_F_000             5041.9034
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6480
_refine_diff_density_min         -0.7048
_refine_diff_density_rms         0.1148
_refine_ls_d_res_high            0.7959
_refine_ls_d_res_low             14.4038
_refine_ls_goodness_of_fit_ref   0.9862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9862
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+9.0839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              28
_reflns_limit_h_min              -31
_reflns_limit_k_max              41
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7822
_reflns_number_total             12740
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc01128e2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        12427.1(16)
_cod_database_code               7123132
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
3. Uiso/Uaniso restraints and constraints
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58)
;
_olex2_submission_special_instructions 'No special instructions were received'