Tris[6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]gadolinium(III) methanol hemisolvate 2.5-hydrate
Kai, Zhao; Yin, Xian-Hong; Yu, Feng; Jie, Zhu; Lin, Cui-Wu; Zhuang, Yue; Acta Crystallographica Section E 64 (2008) m407–m407; doi:10.1107/S1600536808001931

data_2217613
_publ_section_title
;
 Tris[6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]gadolinium(III)
 methanol hemisolvate 2.5-hydrate
;
_journal_coeditor_code           OM2208
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m407
_journal_page_last               m407
_journal_paper_doi               10.1107/S1600536808001931
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Gd (C11 H10 N3 O2)3], 0.5C H4 O, 2.5H2 O'
_chemical_formula_moiety         'C33 H30 N9 Gd O6, 0.5(C H4 O), 2.5(H2 O)'
_chemical_formula_sum            'C33.5 H37 Gd N9 O9'
_chemical_formula_weight         866.97
_chemical_name_systematic
;
Tris[6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]gadolinium(III)
methanol hemisolvate 2.5-hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.434(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5217(18)
_cell_length_b                   16.5515(19)
_cell_length_c                   16.434(2)
_cell_measurement_reflns_used    7251
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.58
_cell_volume                     4028.1(8)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\f and \w'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19991
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.5140
_exptl_absorpt_correction_T_min  0.4826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.003
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                5129
_reflns_number_total             7101
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2208.cif
_cod_data_source_block           I
_cod_original_cell_volume        4028.0(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217613
_cod_database_fobs_code          2217613