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_7121033
_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 Dy3 N16 O46 Zn4, 2(N O3), H3 O'
_chemical_formula_sum            'C72 H79 Dy3 N18 O53 Zn4'
_chemical_formula_weight         2793.51
_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.cc1mkfzl
_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                 94.542(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7456(18)
_cell_length_b                   12.2808(4)
_cell_length_c                   27.4108(12)
_cell_measurement_reflns_used    2594
_cell_measurement_temperature    297.16(10)
_cell_measurement_theta_max      23.3380
_cell_measurement_theta_min      3.6280
_cell_volume                     5619.3(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      297.16(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 0.998
_diffrn_measurement_details
;
  1 omega    3.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000 -150.0000 90

  2 omega  -13.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   19.0000  -30.0000 101

  3 omega    2.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000   90.0000 53
;
_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      -0.0344254000
_diffrn_orient_matrix_UB_12      0.0014521000
_diffrn_orient_matrix_UB_13      -0.0168518000
_diffrn_orient_matrix_UB_21      -0.0241836000
_diffrn_orient_matrix_UB_22      0.0124704000
_diffrn_orient_matrix_UB_23      0.0193487000
_diffrn_orient_matrix_UB_31      0.0062423000
_diffrn_orient_matrix_UB_32      0.0563546000
_diffrn_orient_matrix_UB_33      -0.0038400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_unetI/netI     0.1699
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24643
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.651
_exptl_crystal_F_000             2758
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.635
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         11471
_refine_ls_number_restraints     461
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0843
_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^)+(0.0918P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6021
_reflns_number_total             11471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09092g2.cif
_cod_data_source_block           l-zndy
_cod_depositor_comments
'Adding full bibliography for 7121032--7121033.cif.'
_cod_database_code               7121033
_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, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H,H) groups
2. Restrained distances
 H3-O25
 2 with sigma of 0.02
 H3-O3
 0.8 with sigma of 0.02
 O8-H8
 0.85 with sigma of 0.01
 C26-H8
 1.88881 with sigma of 0.02
 Zn1-H8
 2.878501 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 0.01
4. Rigid body (RIGU) restrains
 N1, N2, N3, N4, N5, N6, N7, N39, N8, O1, O2, O3, O4, O5, O6, O7, O8, O9, O10,
 O11, O12, O13, O14, O15, O16, O17, O18, O19, O20, O21, O22, O23, O24, O25, O26,
  O27, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16,
 C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32,
  C33, C34, C35, C36
 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:
 O20(H20a,H20b), 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              47618
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'