Anion-induced 3d-4f luminescent coordination clusters: structural characteristics and chemical fixation of CO<sub>2</sub> under mild conditions.
Zhang, Ruilian; Wang, Li; Xu, Cong; Yang, Huan; Chen, Wanmin; Gao, Guoshu; Liu, Weisheng; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7159–7165; doi:10.1039/c8dt01292j

data_7046353
_publ_section_title
;
 Anion-induced 3d-4f luminescent coordination clusters: structural
 characteristics and chemical fixation of CO<sub>2</sub> under mild
 conditions.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7159
_journal_page_last               7165
_journal_paper_doi               10.1039/c8dt01292j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38 H42 N4 O30 Tb2 Zn2, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H48 N6 O30 Tb2 Zn2'
_chemical_formula_weight         1565.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1pwphr
_audit_creation_date             2018-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                111.335(5)
_cell_angle_beta                 101.544(7)
_cell_angle_gamma                102.840(6)
_cell_formula_units_Z            1
_cell_length_a                   10.8386(9)
_cell_length_b                   11.0943(5)
_cell_length_c                   13.3764(9)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    290.83(10)
_cell_measurement_theta_max      27.4960
_cell_measurement_theta_min      3.7470
_cell_volume                     1389.11(19)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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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)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -19.00   16.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3041  -99.0000    0.0000 35

  2 omega  -35.00   32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -57.0000 -120.0000 67

  3 omega  -19.00   60.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -99.0000 -180.0000 79

  4 omega  -42.00   42.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -38.0000    0.0000 84

  5 omega    3.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416   57.0000  150.0000 40

  6 omega  -48.00   36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -57.0000  -60.0000 84
;
_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      -0.0243049000
_diffrn_orient_matrix_UB_12      0.0016349000
_diffrn_orient_matrix_UB_13      0.0457670000
_diffrn_orient_matrix_UB_21      0.0659183000
_diffrn_orient_matrix_UB_22      0.0184898000
_diffrn_orient_matrix_UB_23      0.0350427000
_diffrn_orient_matrix_UB_31      0.0067892000
_diffrn_orient_matrix_UB_32      0.0701170000
_diffrn_orient_matrix_UB_33      0.0161604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9549
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82236
_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    1.871
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5447
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0221P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4508
_reflns_number_total             5447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01292j2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7046347--7046353.cif.'
_cod_original_cell_volume        1389.11(17)
_cod_database_code               7046353
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.377
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H8A,H8B,H8C} of C8, {H17A,H17B,H17C} of C17
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H19A,H19B,H19C} of C19, {H21A,H21B,H21C} of C21,
  {H18A,H18B,H18C} of C18
2. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C4(H4), C3(H3), C14(H14), C5(H5)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'