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_7046351
_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         'C48 H56 N2 O36 Tb2 Zn4, 4(C2 H3 N), C2 N'
_chemical_formula_sum            'C58 H68 N7 O36 Tb2 Zn4'
_chemical_formula_weight         2018.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1pwpgq
_audit_creation_date             2018-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-27 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.736(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5467(5)
_cell_length_b                   17.8961(5)
_cell_length_c                   19.5235(5)
_cell_measurement_reflns_used    5289
_cell_measurement_temperature    293.23(10)
_cell_measurement_theta_max      27.8560
_cell_measurement_theta_min      3.6540
_cell_volume                     7739.8(3)
_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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.23(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  -16.00   18.65   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000  -30.0000 33

  2 omega  -52.00   66.65   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -19.0000 -120.0000 113

  3 omega   39.00  102.00   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000  -60.0000 60

  4 omega   65.00   96.50   1.0500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000    0.0000 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      0.0270608000
_diffrn_orient_matrix_UB_12      0.0029789000
_diffrn_orient_matrix_UB_13      -0.0133818000
_diffrn_orient_matrix_UB_21      -0.0036685000
_diffrn_orient_matrix_UB_22      0.0393495000
_diffrn_orient_matrix_UB_23      -0.0022502000
_diffrn_orient_matrix_UB_31      0.0167290000
_diffrn_orient_matrix_UB_32      0.0037081000
_diffrn_orient_matrix_UB_33      0.0343962000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15624
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79492
_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    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             4012
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+19.0238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6182
_reflns_number_total             7597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01292j2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7046347--7046353.cif.'
_cod_database_code               7046351
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O14-N1
 1.5 with sigma of 0.01
 C30A-N4A
 1.1 with sigma of 0.02
 C29-C30A
 1.4 with sigma of 0.02
 H9-O9
 0.95 with sigma of 0.02
 H9-O16
 2.25 with sigma of 0.02
 O18-H9
 2.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30B)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C30A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C30B(0.5) H29D(0.5) H29E(0.5) H29F(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) N4B(0.5) N4A(0.5) C30A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C13(H13), C5(H5), C4(H4), C14(H14)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C29(H29D,H29E,H29F), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'