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_7055466
_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 Gd2 N4 O20), 1.5(H4 O2)'
_chemical_formula_sum            'C28 H54 Gd4 N8 O43'
_chemical_formula_weight         1819.79
_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                73.4450(10)
_cell_angle_beta                 69.8410(10)
_cell_angle_gamma                63.9910(10)
_cell_formula_units_Z            1
_cell_length_a                   10.1500(2)
_cell_length_b                   11.4340(2)
_cell_length_c                   13.5500(2)
_cell_measurement_reflns_used    16673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.91
_cell_measurement_theta_min      27.485
_cell_volume                     1309.92(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 0.994
_diffrn_measured_fraction_theta_max 0.977
_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  0.0715
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25560
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.123
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0032(3)
_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   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0322
_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^)+9.8277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5431
_reflns_number_total             5914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00140h2.cif
_cod_data_source_block           Gdsuc
_cod_depositor_comments
'Adding full bibliography for 7055457--7055469.cif.'
_cod_database_code               7055466
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.361
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  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), C3(H3), C3'(H3')
3.b Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B), O8(H8A,H8B), O11(H11A,H11B), O12(H12A,
 H12B), O13(H13A,H13B), O14(H14A,H14B)
3.d Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
;
_shelx_res_checksum              67086
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'