Homogeneous and silica-supported zinc complexes for the synthesis of propylene carbonate from propane-1,2-diol and carbon dioxide
Comerford, James W.; Hart, Sam J.; North, Michael; Whitwood, Adrian C.; Catal. Sci. Technol. 6 (2016) 4824–; doi:10.1039/C6CY00134C

data_1542538
_publ_section_title
;
 Homogeneous and silica-supported zinc complexes for the synthesis of
 propylene carbonate from propane-1,2-diol and carbon dioxide
;
_journal_issue                   13
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              4824
_journal_paper_doi               10.1039/C6CY00134C
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C23 H32 F3 N8 O3 S Zn, C F3 O3 S'
_chemical_formula_sum            'C24 H32 F6 N8 O6 S2 Zn'
_chemical_formula_weight         772.06
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-01-18 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                68.851(3)
_cell_angle_beta                 81.968(3)
_cell_angle_gamma                82.401(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3731(3)
_cell_length_b                   8.6907(3)
_cell_length_c                   11.7281(5)
_cell_measurement_reflns_used    7999
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.9730
_cell_measurement_theta_min      3.7120
_cell_volume                     785.04(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega    6.00   93.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   57.0000  -60.0000 87

  2 omega    6.00   93.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   57.0000 -120.0000 87

  3 omega   -4.00   94.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   77.0000   30.0000 98

  4 omega  -20.00   65.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712  -99.0000  150.0000 85

  5 omega  -44.00   54.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712  -77.0000  -90.0000 98

  6 omega   -4.00   94.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   77.0000  -60.0000 98

  7 omega -100.00  -55.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -25.4962  178.0000  -30.0000 45

  8 omega  -63.00   47.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -25.4962   19.0000 -120.0000 110

  9 omega    2.00   35.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   37.0000 -180.0000 33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381285000
_diffrn_orient_matrix_UB_12      -0.0273436000
_diffrn_orient_matrix_UB_13      -0.0387238000
_diffrn_orient_matrix_UB_21      -0.0764525000
_diffrn_orient_matrix_UB_22      0.0128411000
_diffrn_orient_matrix_UB_23      0.0314495000
_diffrn_orient_matrix_UB_31      -0.0088418000
_diffrn_orient_matrix_UB_32      0.0824988000
_diffrn_orient_matrix_UB_33      -0.0419349000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14482
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         32.092
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.2125
_exptl_crystal_size_mid          0.1858
_exptl_crystal_size_min          0.0806
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2928 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.037(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8455
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.778
_reflns_Friedel_fraction_max     0.609
_reflns_number_gt                7971
_reflns_number_total             8455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy00134c2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
'Adding full bibliography for 1542536--1542538.cif.'
_cod_database_code               1542538
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H32 F6 N8 O6 S2 Zn1'
_chemical_oxdiff_usercomment     'James C101-B2'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C14(H14), C20(H20)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'