[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_7042680
_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, C6 H2 Cl4 O2, C8 H17 O2, C4 H8 O'
_chemical_formula_sum            'C36 H27 Cl16 O11 P'
_chemical_formula_weight         1233.74
_chemical_name_systematic        H(THF)2[1]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                96.359(6)
_cell_angle_beta                 100.305(5)
_cell_angle_gamma                106.108(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5738(12)
_cell_length_b                   12.1413(13)
_cell_length_c                   17.4244(18)
_cell_measurement_reflns_used    4377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      2.31
_cell_volume                     2280.9(4)
_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  '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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20385
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        23.289
_diffrn_reflns_theta_max         23.289
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0496 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9153. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         6470
_refine_ls_number_restraints     1174
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0348P)^2^+3.4845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4385
_reflns_number_total             6470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04820j2.cif
_cod_data_source_block           dg300_0m_a
_cod_database_code               7042680
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C24-C23 \\sim C24A-C23 \\sim C25-C24A \\sim C25A-C24 \\sim C26A-C25 \\sim
C26-C25A
 with sigma of 0.02
 O7-C22A \\sim O7-C22
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C24A) = Uanis(C24)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H23C)=Sof(H23D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C19A)=Sof(H19C)=
 Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=1-FVAR(2)
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C33(H33A,H33B), C34(H34A,H34B), C23(H23C,
 H23D), C23(H23A,H23B), C21(H21A,H21B), C22(H22A,H22B), C20(H20A,H20B),
 C24A(H24C,H24D), C26A(H26C,H26D), C19(H19A,H19B), C25(H25A,H25B), C21A(H21C,
 H21D), C19A(H19C,H19D), C20A(H20C,H20D), C24(H24A,H24B), C25A(H25C,H25D),
 C26(H26A,H26B), C22A(H22C,H22D)
;
_shelx_res_checksum              83544
_olex2_submission_special_instructions 'No special instructions were received'