Ambient chemical fixation of CO<sub>2</sub> using a highly efficient heterometallic helicate catalyst system.
Wang, Li; Xu, Cong; Han, Qingxin; Tang, Xiaoliang; Zhou, Panpan; Zhang, Ruilian; Gao, Guoshu; Xu, Benhua; Qin, Wenwu; Liu, Weisheng; Chemical communications (Cambridge, England) 54 (2018) 2212–2215; doi:10.1039/c7cc09092g

data_7121032
_publ_section_title
;
 Ambient chemical fixation of CO<sub>2</sub> using a highly efficient
 heterometallic helicate catalyst system.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2212
_journal_page_last               2215
_journal_paper_doi               10.1039/c7cc09092g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C72 H76 N16 O46 Tb3 Zn4, 2(N O3), H3 O'
_chemical_formula_sum            'C72 H79 N18 O53 Tb3 Zn4'
_chemical_formula_weight         2782.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1mkfxj
_audit_creation_date             2016-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-26 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.028(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.310(3)
_cell_length_b                   12.2860(6)
_cell_length_c                   29.5628(16)
_cell_measurement_reflns_used    3114
_cell_measurement_temperature    290.83(10)
_cell_measurement_theta_max      23.2060
_cell_measurement_theta_min      3.6670
_cell_volume                     6149.1(12)
_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  'ShelXL (Sheldrick, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   16.00   85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416   19.0000  -60.0000 69

  2 omega    2.00   28.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416   57.0000  -90.0000 26

  3 omega  -52.00   60.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416    0.0000  -90.0000 112

  4 omega  -20.00   10.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3041  -99.0000 -150.0000 30
;
_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      0.0372864000
_diffrn_orient_matrix_UB_12      -0.0258481000
_diffrn_orient_matrix_UB_13      0.0065667000
_diffrn_orient_matrix_UB_21      0.0055767000
_diffrn_orient_matrix_UB_22      0.0045199000
_diffrn_orient_matrix_UB_23      -0.0230187000
_diffrn_orient_matrix_UB_31      0.0183211000
_diffrn_orient_matrix_UB_32      0.0514111000
_diffrn_orient_matrix_UB_33      0.0053459000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.1780
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            24338
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.303
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69121
_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    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.629
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12519
_refine_ls_number_restraints     889
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1931
_refine_ls_R_factor_gt           0.1293
_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^)+(0.0511P)^2^+266.6821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2756
_refine_ls_wR_factor_ref         0.3156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7186
_reflns_number_total             12519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09092g2.cif
_cod_data_source_block           l-zntb-b
_cod_depositor_comments
'Adding full bibliography for 7121032--7121033.cif.'
_cod_original_cell_volume        6149.3(11)
_cod_database_code               7121032
_reflns_odcompleteness_completeness 99.30
_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) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 N9-O18
 1.2 with sigma of 0.02
 H3-O22
 2.1 with sigma of 0.02
 O3-H3
 0.8 with sigma of 0.02
 H8-O8
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O27(0.5) H27c(0.5) H27d(0.5) H27e(0.5)
6.a Riding coordinates:
 O17(H17a,H17b), O27(H27c,H27d,H27e)
6.b Ternary CH refined with riding coordinates:
 C9(H9), C26(H26)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C10(H10a,H10b), C25(H25a,H25b), C27(H27a,H27b)
6.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C2(H2), C3(H3a), C4(H4a), C5(H5), C11(H11), C15(H15),
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C24(H24), C30(H30), C31(H31),
  C32(H32), C33(H33)
6.e Idealised Me refined as rotating group:
 C35(H35a,H35b,H35c), C36(H36a,H36b,H36c)
;
_shelx_fab_checksum              8162
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'