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_7231688
_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 N18 Nd4 O42 Zn3, 6(C2 H3 N)'
_chemical_formula_sum            'C114 H126 N24 Nd4 O42 Zn3'
_chemical_formula_weight         3277.45
_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                   17.8928(5)
_cell_length_b                   17.8928(5)
_cell_length_c                   69.099(2)
_cell_measurement_reflns_used    3865
_cell_measurement_temperature    290.83(10)
_cell_measurement_theta_max      23.7250
_cell_measurement_theta_min      3.4900
_cell_volume                     19158.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  25.00   0.50   12.50    --  -17.15 -99.00  60.00   56
  2  \w     39.00  77.00   0.50   12.50    --   20.59  38.00 120.00   76
  3  \w    -47.00  20.00   0.50   12.50    --   20.59 -57.00 150.00  134
  4  \w    -16.00  54.00   0.50   12.50    --   20.59 -99.00-120.00  140
  5  \w    -22.00  41.00   0.50   12.50    --   20.59 -57.00 -90.00  126
  6  \w     -4.00  80.50   0.50   12.50    --   20.59  77.00  30.00  169
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284225000
_diffrn_orient_matrix_UB_12      0.0077243000
_diffrn_orient_matrix_UB_13      0.0078708000
_diffrn_orient_matrix_UB_21      0.0146575000
_diffrn_orient_matrix_UB_22      0.0448168000
_diffrn_orient_matrix_UB_23      -0.0005814000
_diffrn_orient_matrix_UB_31      -0.0327569000
_diffrn_orient_matrix_UB_32      -0.0052644000
_diffrn_orient_matrix_UB_33      0.0065656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            43234
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.856
_diffrn_reflns_theta_min         3.491
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             9864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.971
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5402
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+75.9280P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2954
_reflns_number_total             5402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc02645a2.cif
_cod_data_source_block           l-znnd
_cod_original_cell_volume        19158.4(12)
_cod_database_code               7231688
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.63
_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(C19) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O6(H6A,H6B)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C2(H2), C5(H5), N2(H2A), C4(H4), C16(H16), C13(H13), C10(H10)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              53176
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.832