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_7225470
_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         'C17 H16 Br2 Cu2 N2 O7 Tb, O'
_chemical_formula_sum            'C17 H16 Br2 Cu2 N2 O8 Tb'
_chemical_formula_weight         822.15
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_date             2016-05-28
_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                86.456(3)
_cell_angle_beta                 87.677(4)
_cell_angle_gamma                65.171(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4069(15)
_cell_length_b                   7.7788(15)
_cell_length_c                   21.614(4)
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.904
_cell_measurement_theta_min      1.888
_cell_volume                     1127.9(4)
_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 0.989
_diffrn_measured_fraction_theta_max 0.898
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6718
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.904
_diffrn_reflns_theta_min         1.888
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.181
_exptl_transmission_factor_min   0.140
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3219
_reflns_number_total             5396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00637j2.cif
_cod_data_source_block           17
_cod_depositor_comments
'Adding full bibliography for 7225454--7225470.cif.'
_cod_database_code               7225470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H,H) groups
2. Restrained distances
 O1W-H1W = O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1W-H1WA = H1W-H1WB
 1.39 with sigma of 0.01
 H1W-Tb1 \\sim H1WA-Tb1 \\sim H1WB-Tb1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2W \\sim O2B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O2B)=1-FVAR(1)
 Sof(O2W)=FVAR(1)
 Fixed Sof: H1WA(0.5) H1WB(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              29647
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'