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_1542536
_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         'C22 H16 F6 N4 O6 S2 Zn'
_chemical_formula_sum            'C22 H16 F6 N4 O6 S2 Zn'
_chemical_formula_weight         675.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-01-18
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2016-01-18 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5148(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.92044(14)
_cell_length_b                   14.02733(18)
_cell_length_c                   18.6185(3)
_cell_measurement_reflns_used    8909
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      32.0180
_cell_measurement_theta_min      3.6490
_cell_volume                     2538.75(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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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 0.997
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
  1 omega  -46.00   47.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712  -37.0000  -90.0000 93

  2 omega  -47.00   63.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712  -19.0000    0.0000 110

  3 omega   -4.00   94.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   77.0000 -120.0000 98

  4 omega   35.00   99.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712  178.0000  -90.0000 64

  5 omega    6.00   59.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   57.0000    0.0000 53

  6 omega    6.00   93.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8712   57.0000   60.0000 87
;
_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      -0.0647743000
_diffrn_orient_matrix_UB_12      -0.0206085000
_diffrn_orient_matrix_UB_13      0.0013114000
_diffrn_orient_matrix_UB_21      0.0293274000
_diffrn_orient_matrix_UB_22      -0.0230901000
_diffrn_orient_matrix_UB_23      0.0333469000
_diffrn_orient_matrix_UB_31      -0.0164052000
_diffrn_orient_matrix_UB_32      0.0399864000
_diffrn_orient_matrix_UB_33      0.0199405000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16102
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.163
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.2637
_exptl_crystal_size_mid          0.2049
_exptl_crystal_size_min          0.1378
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0276P)^2^+3.0392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3763
_reflns_number_total             4183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy00134c2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 1542536--1542538.cif.'
_cod_database_code               1542536
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C22 H16 F6 N4 O6 S2 Zn1'
_chemical_oxdiff_usercomment     'James's C101-B1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_olex2_date_sample_data_collection 1409219341.36
_olex2_submission_special_instructions 'No special instructions were received'