Topologically diverse shape-persistent bis-(Zn-salphen) catalysts: efficient cyclic carbonate formation under mild conditions.
He, Shixiong; Wang, Fuli; Tong, Wah-Leung; Yiu, Shek-Man; Chan, Michael C. W.; Chemical communications (Cambridge, England) 52 (2016) 1017–1020; doi:10.1039/c5cc08794e

data_7118335
_publ_section_title
;
 Topologically diverse shape-persistent bis-(Zn-salphen) catalysts:
 efficient cyclic carbonate formation under mild conditions.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1017
_journal_page_last               1020
_journal_paper_doi               10.1039/c5cc08794e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '0.5(C140 H136 N8 O14 Zn4)'
_chemical_formula_sum            'C70 H68 N4 O7 Zn2'
_chemical_formula_weight         1208.02
_chemical_name_systematic        7?AcOH
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Aug 16 09:53:59 2013'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record
;
2015-06-17 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   17.8685(2)
_cell_length_b                   23.0557(2)
_cell_length_c                   18.5326(2)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5238
_cell_measurement_theta_min      3.0568
_cell_volume                     7634.89(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -20.00    6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -150.0000 26

  2 omega   14.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 50

  3 omega  -12.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -111.0000  148.0000 61

  4 omega   73.00  123.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -60.0000 50

  5 omega -140.00  -80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 60

  6 omega  -71.00    6.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  -30.0000 77

  7 omega   40.00   82.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   30.0000 42

  8 omega   37.00   69.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 32

  9 omega   45.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 26

 10 omega   38.00  116.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 78

 11 omega   38.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 25

 12 omega   38.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 25

 13 omega   44.00   69.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 25

 14 omega   37.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 31

 15 omega   38.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 30

 16 omega   53.00   79.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  150.0000 26

 17 omega   41.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 29

 18 omega  -30.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -30.0000 100

 19 omega    8.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -143.0000 -133.0000 61

 20 omega  -26.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000 -120.0000 98

 21 omega -125.00  -25.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -77.0000  -60.0000 100

 22 omega   80.00  162.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000 -150.0000 82
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0150804000
_diffrn_orient_matrix_UB_12      -0.0179600000
_diffrn_orient_matrix_UB_13      0.0787840000
_diffrn_orient_matrix_UB_21      -0.0096154000
_diffrn_orient_matrix_UB_22      0.0642226000
_diffrn_orient_matrix_UB_23      0.0209596000
_diffrn_orient_matrix_UB_31      -0.0842997000
_diffrn_orient_matrix_UB_32      -0.0041341000
_diffrn_orient_matrix_UB_33      -0.0164702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31864
_diffrn_reflns_theta_full        71.72
_diffrn_reflns_theta_max         71.72
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethyl acetate'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7390
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+1.7271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                5456
_reflns_number_total             7390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc08794e2.cif
_cod_data_source_block           081513a_shixiong
_cod_original_cell_volume        7634.92(15)
_cod_database_code               7118335
_cell_oxdiff_angle_alpha         89.991(3)
_cell_oxdiff_angle_beta          89.991(2)
_cell_oxdiff_angle_gamma         90.018(2)
_cell_oxdiff_length_a            17.8769(5)
_cell_oxdiff_length_b            23.0572(7)
_cell_oxdiff_length_c            18.5227(6)
_cell_oxdiff_measurement_reflns_used 8826
_cell_oxdiff_volume              7634.9(4)
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13