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_1542537
_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         'C26 H16 F6 N4 O6 S2 Zn'
_chemical_formula_sum            'C26 H16 F6 N4 O6 S2 Zn'
_chemical_formula_weight         723.92
_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                 95.2384(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.75476(12)
_cell_length_b                   14.26536(17)
_cell_length_c                   19.5942(2)
_cell_measurement_reflns_used    6506
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.9100
_cell_measurement_theta_min      3.8750
_cell_volume                     2715.25(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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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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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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_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 0.922
_diffrn_measurement_details
;
  1 omega   -4.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7780   77.0000 -150.0000 98

  2 omega   -2.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7780   73.0000  102.0000 95

  3 omega   35.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7780  178.0000 -120.0000 64

  4 omega  -44.00   53.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7780  -77.0000   90.0000 97

  5 omega   34.00   59.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7780 -178.0000    0.0000 25
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_21      -0.0219415000
_diffrn_orient_matrix_UB_22      0.0395247000
_diffrn_orient_matrix_UB_23      0.0180890000
_diffrn_orient_matrix_UB_31      -0.0629991000
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_diffrn_orient_matrix_UB_33      -0.0211614000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12898
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.080
_diffrn_reflns_theta_min         3.402
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   analytical
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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    1.771
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_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2088
_exptl_crystal_size_mid          0.1305
_exptl_crystal_size_min          0.1221
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_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0329P)^2^+2.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0722
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_reflns_number_gt                3895
_reflns_number_total             4395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy00134c2.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 1542536--1542538.cif.'
_cod_original_cell_volume        2715.24(6)
_cod_database_code               1542537
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C22 H16 F6 N4 O6 S2 Zn1'
_chemical_oxdiff_usercomment     'James C101-B3'
_reflns_odcompleteness_completeness 99.69
_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), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
;
_olex2_date_sample_data_collection 1409666177.15
_olex2_submission_special_instructions 'No special instructions were received'