Rare earth coordination dinuclear compounds constructed from 3,5-dicarboxypyrazolate and succinate intermetallic bridges
Lahoud, Marcelo G.; Muniz, Elaine C.; Arroyos, Guilherme; Fávaro, Marcelo A.; Davolos, Marian R.; D'Vries, Richard F.; Ellena, Javier; Freitas, Rafael S.; Arrighi, Everton; Frem, Regina C. G.; New J. Chem. 40 (2016) 5338–; doi:10.1039/C6NJ00140H

data_7055469
_publ_section_title
;
 Rare earth coordination dinuclear compounds constructed from
 3,5-dicarboxypyrazolate and succinate intermetallic bridges
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              5338
_journal_paper_doi               10.1039/C6NJ00140H
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '2(C14 H24 Ce2 N4 O20), 3(H2 O)'
_chemical_formula_sum            'C28 H54 Ce4 N8 O43'
_chemical_formula_weight         1751.27
_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             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-30 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                73.7490(10)
_cell_angle_beta                 70.1140(10)
_cell_angle_gamma                64.0920(10)
_cell_formula_units_Z            1
_cell_length_a                   10.2740(2)
_cell_length_b                   11.56400(10)
_cell_length_c                   13.6900(2)
_cell_measurement_reflns_used    16909
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1359.13(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      293.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31802
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         3.496
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_description       prism
_exptl_crystal_F_000             854
_exptl_crystal_preparation       'Magnetic properties, Luminescent'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0059(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0612P)^2^+1.6182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5520
_reflns_number_total             6112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00140h2.cif
_cod_data_source_block           Cesuc
_cod_depositor_comments
'Adding full bibliography for 7055457--7055469.cif.'
_cod_database_code               7055469
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.373
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Riding coordinates:
 N1'(H1'), N1(H1), O6(H6A,H6B), O7(H7A,H7B), O8(H8A,H8B), O12(H12A,H12B),
 O14(H14A,H14B), O2W(H2WA,H2WB)
3.b Free rotating group:
 O1W(H1WA,H1WB)
3.c Rotating group:
 O5(H5A,H5B), O11(H11A,H11B), O13(H13A,H13B)
3.d Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
3.e Aromatic/amide H refined with riding coordinates:
 C3'(H3'), C3(H3)
;
_shelx_res_checksum              62912
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'