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_4505941
_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         'C38 H52 N14 Ni2 O8, 3(C3 H7 N O), 2(N O3)'
_chemical_formula_sum            'C47 H73 N19 Ni2 O17'
_chemical_formula_weight         1293.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.960(4)
_cell_angle_beta                 95.722(5)
_cell_angle_gamma                103.508(5)
_cell_formula_units_Z            1
_cell_length_a                   10.1334(12)
_cell_length_b                   13.8385(6)
_cell_length_c                   13.9286(6)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      25.426
_cell_measurement_theta_min      2.215
_cell_volume                     1661.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16858
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.9270
_exptl_absorpt_correction_T_min  0.8879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2351
_reflns_number_gt                5896
_reflns_number_total             7912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201677s_si_002.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505941