#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:40:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178819 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/73/4107309.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4107309
loop_
_publ_author_name
'Jie-Peng Zhang'
'Susumu Kitagawa'
_publ_section_title
;
 Supramolecular Isomerism, Framework Flexibility, Unsaturated Metal
 Center, and Porous Property of Ag(I)/Cu(I)
 3,3',5,5'-Tetrametyl-4,4'-Bipyrazolate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              907
_journal_page_last               917
_journal_paper_doi               10.1021/ja075408b
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C10 H12 Cu2 N4'
_chemical_formula_weight         315.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            48
_cell_length_a                   26.407(3)
_cell_length_b                   26.407(3)
_cell_length_c                   26.407(3)
_cell_measurement_temperature    373(2)
_cell_volume                     18414(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '/w scan'
_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  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29240
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.6090
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   REQABA
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       colorless
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0550P)²+160.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                1467
_reflns_number_total             2816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075408b-file006.cif
_cod_data_source_block           1-Cu
_cod_original_cell_volume        18415(4)
_cod_database_code               4107309
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.42337(7) 0.98434(7) 0.00135(7) 0.1029(6) Uani 1 1 d .
Cu2 Cu 0.23233(7) 1.14869(7) 0.23430(7) 0.1042(6) Uani 1 1 d .
N1 N 0.4109(6) 1.0320(5) 0.0517(5) 0.120(5) Uani 1 1 d .
N2 N 0.4471(5) 1.0691(6) 0.0597(5) 0.111(4) Uani 1 1 d .
C1 C 0.3243(6) 1.0125(6) 0.0714(7) 0.129(6) Uani 1 1 d .
H1A H 0.3179 1.0050 0.0364 0.193 Uiso 1 1 calc R
H1B H 0.2957 1.0300 0.0855 0.193 Uiso 1 1 calc R
H1C H 0.3297 0.9815 0.0896 0.193 Uiso 1 1 calc R
C2 C 0.3702(7) 1.0449(7) 0.0755(6) 0.108(5) Uani 1 1 d .
C3 C 0.3744(7) 1.0922(7) 0.0982(7) 0.121(5) Uani 1 1 d .
C4 C 0.4266(9) 1.1061(6) 0.0875(7) 0.132(7) Uani 1 1 d .
C5 C 0.4565(6) 1.1508(6) 0.1012(6) 0.123(6) Uani 1 1 d .
H5A H 0.4354 1.1803 0.0998 0.185 Uiso 1 1 calc R
H5B H 0.4841 1.1545 0.0779 0.185 Uiso 1 1 calc R
H5C H 0.4695 1.1467 0.1349 0.185 Uiso 1 1 calc R
N3 N 0.2843(5) 1.1469(5) 0.1874(6) 0.116(4) Uani 1 1 d .
N4 N 0.2854(6) 1.1842(6) 0.1501(6) 0.127(5) Uani 1 1 d .
C6 C 0.3240(6) 1.0633(6) 0.2038(6) 0.129(6) Uani 1 1 d .
H6A H 0.3258 1.0728 0.2388 0.194 Uiso 1 1 calc R
H6B H 0.3557 1.0486 0.1936 0.194 Uiso 1 1 calc R
H6C H 0.2973 1.0391 0.1991 0.194 Uiso 1 1 calc R
C7 C 0.3137(6) 1.1092(6) 0.1723(6) 0.101(4) Uani 1 1 d .
C8 C 0.3378(6) 1.1234(7) 0.1257(7) 0.113(5) Uani 1 1 d .
C9 C 0.3181(6) 1.1711(7) 0.1134(8) 0.117(5) Uani 1 1 d .
C10 C 0.3276(7) 1.2045(6) 0.0713(6) 0.126(5) Uani 1 1 d .
H10A H 0.3173 1.2382 0.0801 0.189 Uiso 1 1 calc R
H10B H 0.3087 1.1932 0.0424 0.189 Uiso 1 1 calc R
H10C H 0.3631 1.2043 0.0635 0.189 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Cu1 N1 174.1(6) 12_664 .
N3 Cu2 N4 175.3(6) . 9_465
C2 N1 N2 108.3(15) . .
C2 N1 Cu1 132.4(15) . .
N2 N1 Cu1 117.8(12) . .
C4 N2 N1 108.8(14) . .
C4 N2 Cu1 125.2(14) . 6_566
N1 N2 Cu1 120.9(12) . 6_566
N1 C2 C3 112.4(17) . .
N1 C2 C1 119.4(18) . .
C3 C2 C1 127.8(16) . .
C2 C3 C4 102.6(16) . .
C2 C3 C8 131.9(17) . .
C4 C3 C8 125.5(17) . .
N2 C4 C3 107.8(15) . .
N2 C4 C5 121(2) . .
C3 C4 C5 132(2) . .
C7 N3 N4 107.9(14) . .
C7 N3 Cu2 131.1(12) . .
N4 N3 Cu2 118.0(11) . .
C9 N4 N3 109.9(15) . .
C9 N4 Cu2 129.0(14) . 5_564
N3 N4 Cu2 119.0(11) . 5_564
N3 C7 C8 108.8(15) . .
N3 C7 C6 123.3(15) . .
C8 C7 C6 127.4(15) . .
C9 C8 C7 105.6(17) . .
C9 C8 C3 129.6(19) . .
C7 C8 C3 124.9(16) . .
N4 C9 C8 107.6(18) . .
N4 C9 C10 120.7(17) . .
C8 C9 C10 132(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.855(13) 12_664
Cu1 N1 1.859(14) .
Cu2 N3 1.851(13) .
Cu2 N4 1.855(17) 9_465
N1 C2 1.292(18) .
N1 N2 1.384(18) .
N2 C4 1.34(2) .
N2 Cu1 1.855(13) 6_566
C1 C2 1.49(2) .
C2 C3 1.39(2) .
C3 C4 1.46(3) .
C3 C8 1.46(2) .
C4 C5 1.46(2) .
N3 C7 1.322(17) .
N3 N4 1.393(18) .
N4 C9 1.34(2) .
N4 Cu2 1.855(17) 5_564
C6 C7 1.49(2) .
C7 C8 1.43(2) .
C8 C9 1.40(2) .
C9 C10 1.44(2) .
