[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_7042679
_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, 1.53(C3 H6 O0.75), 3.1(C2 H3 N)'
_chemical_formula_sum            'C28.8 H18.5 Cl12 N3.11 O7.15 P'
_chemical_formula_weight         978.87
_chemical_name_systematic        H(CH3CN)(THF)[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     direct
_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                66.919(5)
_cell_angle_beta                 83.382(6)
_cell_angle_gamma                84.392(5)
_cell_formula_units_Z            2
_cell_length_a                   11.823(3)
_cell_length_b                   12.984(3)
_cell_length_c                   14.193(3)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.43
_cell_volume                     1987.7(8)
_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      90(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 0.995
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40251
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.158
_diffrn_reflns_theta_min         1.708
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0503 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.9118.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       plate
_exptl_crystal_F_000             979
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.713
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         11706
_refine_ls_number_restraints     752
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+4.3861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9008
_reflns_number_total             11706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04820j2.cif
_cod_data_source_block           dg333_a
_cod_original_cell_volume        1987.8(7)
_cod_original_formula_sum        'C28.80 H18.50 Cl12 N3.11 O7.15 P'
_cod_database_code               7042679
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N100-C1AA
 2.6 with sigma of 0.01
 C25-C26 = C27-C26 = C27-C28A
 1.535 with sigma of 0.01
 N4-C1A \\sim N100-C2AA
 with sigma of 0.01
 C1B-C1A \\sim C2AA-C1AA
 with sigma of 0.01
 O8A-C25 \\sim O7-C25 \\sim O8A-C28A \\sim O7-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O8 \\sim N4 \\sim C1A \\sim C1B \\sim C1E \\sim H1EA \\sim C1F \\sim H1BA \\sim
H1BB \\sim H1BC \\sim C1D \\sim H1EB \\sim H1FA \\sim H1FB \\sim C1C \\sim C1AA
\\sim H1AC \\sim C2AA \\sim H1DA \\sim H1DB \\sim H1CA \\sim H1CB \\sim H1AA
\\sim H1AB \\sim N100: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O7) = Uanis(O8A)
Uanis(C19) = Uanis(C19A)
Uanis(N1A) = Uanis(N1)
Uanis(C1A) = Uanis(N100)
Uanis(C28) = Uanis(C28A)
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
 1*[Sof(O8)+Sof(C1C)+Sof(H1CA)+Sof(H1CB)+Sof(C1D)+Sof(H1DA)+Sof(H1DB)+Sof(C1E)+
 Sof(H1EA)+Sof(H1EB)+Sof(C1F)+Sof(H1FA)+Sof(H1FB)]+1*[Sof(N4)+Sof(C1A)+Sof(C1B)+
 Sof(H1BA)+Sof(H1BB)+Sof(H1BC)]+1*[Sof(C1AA)+Sof(H1AA)+Sof(H1AB)+Sof(H1AC)+
 Sof(C2AA)+Sof(N100)]=1 with esd of 0.002
 Sof(O8A)=Sof(H25C)=Sof(H25D)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28C)=
 Sof(H28D)=0.75*(1-FVAR(2))
 Sof(O7)=Sof(H25A)=Sof(H25B)=Sof(H27C)=Sof(H27D)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 0.75*FVAR(2)
 Sof(N1A)=Sof(C19A)=1-FVAR(2)
 Sof(C19)=Sof(N1)=FVAR(2)
 Sof(O8)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(C1E)=
 Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=FVAR(3)
 Sof(N4)=Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=FVAR(4)
 Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2AA)=Sof(N100)=FVAR(5)
 Fixed Sof: C25(0.75) C26(0.75) H26A(0.75) H26B(0.75) C27(0.75) N3(0.5)
 C23(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 Fixed X: H20A(0.414889) H20B(0.285089) H20C(0.346089)
 Fixed Y: H20A(0.616381) H20B(0.65513) H20C(0.612061)
 Fixed Z: H20A(0.41717) H20B(0.417729) H20C(0.51978)
6.a Free rotating group:
 N3(C23,C24), N4(C1A,C1B), O8(C1C,C1D,C1E,C1F)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B), C27(H27C,H27D), C27(H27A,
 H27B), C28(H28A,H28B), C28A(H28C,H28D), C1C(H1CA,H1CB), C1D(H1DA,H1DB),
 C1E(H1EA,H1EB), C1F(H1FA,H1FB)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C1B(H1BA,H1BB,H1BC), C1AA(H1AA,H1AB,
 H1AC)
;
_shelx_res_checksum              1115
_olex2_submission_special_instructions 'No special instructions were received'