Pyrazolate-based copper(II) and nickel(II) [2 x 2] grid complexes: protonation-dependent self-assembly, structures and properties.
Klingele, Julia; Prikhod'ko, Alexander I.; Leibeling, Guido; Demeshko, Serhiy; Dechert, Sebastian; Meyer, Franc; Dalton transactions (Cambridge, England : 2003)  (2007) 2003–2013; doi:10.1039/b701981e

data_7005404
_publ_section_title
;
 Pyrazolate-based copper(II) and nickel(II) [2 x 2] grid complexes:
 protonation-dependent self-assembly, structures and properties.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2003
_journal_page_last               2013
_journal_paper_doi               10.1039/b701981e
_journal_year                    2007
_chemical_formula_moiety         'C17 H16 N6 O2, 2(H2 O)'
_chemical_formula_sum            'C17 H20 N6 O4'
_chemical_formula_weight         372.39
_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                66.677(4)
_cell_angle_beta                 78.628(4)
_cell_angle_gamma                72.036(4)
_cell_formula_units_Z            4
_cell_length_a                   11.9866(6)
_cell_length_b                   12.5344(6)
_cell_length_c                   13.7972(7)
_cell_measurement_reflns_used    40196
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      1.61
_cell_volume                     1804.07(17)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40196
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0552P)^2^+0.3393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                5284
_reflns_number_total             6177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701981e.txt
_cod_data_source_block           H3L
_cod_original_cell_volume        1804.07(15)
_cod_database_code               7005404