[HL2][P(1,2-O2C6Cl4)3] (L = THF, DMF): Brønsted acid initiators for the polymerization of n-butyl vinyl ether and p-methoxystyrene
Hazin, Khatera; Serin, Spencer C.; Patrick, Brian O.; Ezhova, Maria B.; Gates, Derek P.; Dalton Trans.  (2017) –; doi:10.1039/C6DT04820J

data_7042681
_publ_section_title
;
 [HL2][P(1,2-O2C6Cl4)3] (L = THF, DMF): Br\/onsted acid initiators for the
 polymerization of n-butyl vinyl ether and p-methoxystyrene
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04820J
_journal_year                    2017
_chemical_formula_moiety         'C18 Cl12 O6 P, 2(C3 H7 N O), 0.2(C H2 Cl2)'
_chemical_formula_sum            'C24.2 H14.4 Cl12.4 N2 O8 P'
_chemical_formula_weight         931.73
_chemical_name_systematic        H(DMF)2[1]
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.450(2)
_cell_angle_gamma                90
_cell_formula_units_Z            20
_cell_length_a                   40.2932(19)
_cell_length_b                   26.2969(12)
_cell_length_c                   16.7720(8)
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.60
_cell_volume                     17209.2(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            132635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.967
_diffrn_reflns_theta_min         0.934
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0648 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.8856. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       prism
_exptl_crystal_F_000             9268
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2164
_refine_ls_number_reflns         40536
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0543P)^2^+112.6505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                36389
_reflns_number_total             40536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04820j2.cif
_cod_data_source_block           dg204
_cod_original_formula_sum        'C24.20 H14.40 Cl12.40 N2 O8 P'
_cod_database_code               7042681
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.633
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(5)
 0.14(5)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C118(H11S,H11T)
3.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C106(H106), C100(H100), C109(H109), C97(H97), C112(H112),
 C94(H94), C115(H115), C06A(H06A), C91(H91)
3.c Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C105(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,
 H10K,H10L), C101(H10M,H10N,H10O), C102(H10P,H10Q,H10R), C110(H11A,H11B,H11C),
 C111(H11D,H11E,H11F), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C113(H11G,H11H,
 H11I), C114(H11J,H11K,H11L), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C),
 C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R), C0AA(H0AA,H0AB,H0AC), C06H(H06B,
 H06C,H06D), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C)
;
_shelx_res_checksum              71703
_olex2_submission_special_instructions 'No special instructions were received'