Three types of lanthanide coordination polymers from 1D to 3D based on a tetracarboxylate ligand: synthesis, structural diversities and properties
Du, Pei-Yao; Gu, Wen; Liu, Xin; CrystEngComm 18 (2016) 5140–; doi:10.1039/C6CE00600K

data_7225255
_publ_section_title
;
 Three types of lanthanide coordination polymers from 1D to 3D based on a
 tetracarboxylate ligand: synthesis, structural diversities and properties
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5140
_journal_paper_doi               10.1039/C6CE00600K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C34 H36 Gd N5 O22'
_chemical_formula_weight         1023.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6624(15)
_cell_length_b                   21.609(4)
_cell_length_c                   12.271(3)
_cell_measurement_reflns_used    5902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9704
_cell_measurement_theta_min      1.6792
_cell_volume                     2007.9(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15982
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The SQUEEZE routine of PLATON was applied to remove the diffraction contribution from guests to give a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 152 electrons per unit cell. This corresponds with 152/4=38 electrons per asymmetric unit. As the formula unit is composed of 2 asymmetric units (Z = 2), this then implies that 76 electrons removed by SQUEEZE should be associated with the formula unit. As there are 10 electrons with a water molecule, the logical deduction is that some 7.6 water molecules should be added to the formula unit. The remaining solvent molecules were disordered and assigned as five H2O molecule according to the TGA and elemental analysis results, as the formula unit. This discrepancy might be owing to the moderate quality of low angle data caused by the highly disordered framework.
;
_refine_diff_density_max         5.652
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1353P)^2^+23.9214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2311
_reflns_number_gt                3170
_reflns_number_total             3630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00600k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7225253--7225260.cif.
;
_cod_original_cell_volume        2008.0(7)
_cod_original_sg_symbol_H-M      p21/m
_cod_database_code               7225255