Polynuclear Complexes Containing Ditopic Bispyrazolylmethane Ligands. Influence of Metal Geometry and Supramolecular Interactions
Carrión, M. Carmen; Durá, Gema; Jalón, Félix A.; Manzano, Blanca R.; Rodríguez, Ana M.; Crystal Growth & Design 12 (2012) 1952–; doi:10.1021/cg201677s

data_4505937
_publ_section_title
;
 Polynuclear Complexes Containing Ditopic Bispyrazolylmethane Ligands.
 Influence of Metal Geometry and Supramolecular Interactions
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1952
_journal_paper_doi               10.1021/cg201677s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C36 H43 N10 Pd3, 3(B F4)'
_chemical_formula_sum            'C36 H43 B3 F12 N10 Pd3'
_chemical_formula_weight         1195.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.883(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.949(3)
_cell_length_b                   26.138(6)
_cell_length_c                   16.170(3)
_cell_measurement_reflns_used    2687
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      19.855
_cell_measurement_theta_min      2.342
_cell_volume                     4923.1(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37068
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.9023
_exptl_absorpt_correction_T_min  0.8175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                5326
_reflns_number_total             8671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201677s_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        4923.4(19)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4505937