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_7123131
_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         'C29 H24 O3 P V'
_chemical_formula_sum            'C29 H24 O3 P V'
_chemical_formula_weight         502.43
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2018-07-14
_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                 97.09(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.190(8)
_cell_length_b                   11.081(9)
_cell_length_c                   21.340(19)
_cell_measurement_reflns_used    1734
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.66
_cell_volume                     2391(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  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      107.05
_diffrn_measured_fraction_theta_full 0.9759
_diffrn_measured_fraction_theta_max 0.9759
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15809
_diffrn_reflns_theta_full        27.1466
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1254 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.6419.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.3956
_exptl_crystal_description       'blue plate'
_exptl_crystal_F_000             1042.1107
_refine_diff_density_max         0.6643
_refine_diff_density_min         -1.1034
_refine_diff_density_rms         0.1884
_refine_ls_d_res_high            0.7789
_refine_ls_d_res_low             10.5882
_refine_ls_goodness_of_fit_ref   0.8971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8971
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.2280
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2614
_reflns_number_total             5178
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc01128e2.cif
_cod_data_source_block           final_a
_cod_original_cell_volume        2391(4)
_cod_database_code               7123131
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C00A(H00A), C00B(H00B), C00D(H00D), C00F(H00F), C00G(H00G),
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y)
;
_olex2_submission_special_instructions 'No special instructions were received'