Copper(i)‒lanthanide(iii) heterometallic metal‒organic frameworks constructed from 3-(3-pyridyl)acrylic acid: syntheses, structures, and properties
Dong, Ruo-Ting; Chen, Xin-Li; Cui, Xiao; Chen, Su-Su; Shen, Mo-Yuan; Li, Chu-Wen; Li, Qian-Hong; Hu, Ming-Yuan; Huang, Lan-Fen; Deng, Hong; CrystEngComm 18 (2016) 5547–; doi:10.1039/C6CE00637J

data_7225461
_publ_section_title
;
 Copper(i)--lanthanide(iii) heterometallic metal--organic frameworks
 constructed from 3-(3-pyridyl)acrylic acid: syntheses, structures, and
 properties
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5547
_journal_paper_doi               10.1039/C6CE00637J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.25(C192 H176 Cu8 I8 N24 O64 Tb8), H2 O'
_chemical_formula_sum            'C48 H46 Cu2 I2 N6 O17 Tb2'
_chemical_formula_weight         1677.67
_chemical_name_systematic
;
 ?
;
_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_creation_date             2016-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.5140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9956(15)
_cell_length_b                   9.2876(6)
_cell_length_c                   29.387(3)
_cell_measurement_reflns_used    6757
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.947
_cell_measurement_theta_min      1.977
_cell_volume                     5622.7(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.977
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.402
_exptl_absorpt_correction_T_max  0.415
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4852
_reflns_number_total             6486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00637j2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7225454--7225470.cif.'
_cod_original_cell_volume        5622.7(7)
_cod_database_code               7225461
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O3B-H3BA = O3B-H3BB = O1W-H1WA = O1W-H1WB = O2W-H2WA =
 O2W-H2WB
 0.82 with sigma of 0.01
 H3WA-H3WB = H3BA-H3BB = H1WA-H1WB = H2WA-H2WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3W \\sim O3B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O3B)=Sof(H3BA)=Sof(H3BB)=0.5*(1-FVAR(2))
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_shelx_res_checksum              23609
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'