Amide-functionalized heterometallic helicate cages as highly efficient catalysts for CO2 conversion under mild condition
Wang, Li; Zhang, Ruilian; Han, Qing-Xin; Xu, Cong; Chen, Wan-Min; Yang, Huan; Gao, Guoshu; Qin, Wenwu; Liu, Wei-Sheng; Green Chemistry  (2018) –; doi:10.1039/C8GC02645A

data_7231689
_publ_section_title
;
 Amide-functionalized heterometallic helicate cages as highly efficient
 catalysts for CO2 conversion under mild condition
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/C8GC02645A
_journal_year                    2018
_chemical_formula_moiety         'C102 H108 Eu4 N18 O42 Zn3, 6(C2 H3 N)'
_chemical_formula_sum            'C114 H126 Eu4 N24 O42 Zn3'
_chemical_formula_weight         3308.33
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-12 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.8497(5)
_cell_length_b                   17.8497(5)
_cell_length_c                   68.762(2)
_cell_measurement_reflns_used    10511
_cell_measurement_temperature    290.83(10)
_cell_measurement_theta_max      24.7600
_cell_measurement_theta_min      3.4970
_cell_volume                     18973.2(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.83(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -1.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   57.0000   90.0000 88

  2 omega   61.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   77.0000    0.0000 30

  3 omega   39.00   83.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  178.0000 -120.0000 44

  4 omega   -3.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   38.0000    0.0000 96

  5 omega  -18.00    9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  -30.0000 27

  6 omega  -40.00   35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -57.0000 -150.0000 75

  7 omega  -20.00    8.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  120.0000 28
;
_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      -0.0166591000
_diffrn_orient_matrix_UB_12      0.0011375000
_diffrn_orient_matrix_UB_13      -0.0092940000
_diffrn_orient_matrix_UB_21      0.0082059000
_diffrn_orient_matrix_UB_22      0.0425139000
_diffrn_orient_matrix_UB_23      0.0018980000
_diffrn_orient_matrix_UB_31      0.0419540000
_diffrn_orient_matrix_UB_32      0.0172320000
_diffrn_orient_matrix_UB_33      -0.0040564000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            42103
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         3.496
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.800
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4145
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0261P)^2^+230.4551P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2609
_reflns_number_total             4145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc02645a2.cif
_cod_data_source_block           l-zneu
_cod_original_cell_volume        18973.1(12)
_cod_database_code               7231689
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.64
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C17(H17), C13(H13), C10(H10)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              65407
_olex2_submission_special_instructions 'No special instructions were received'