#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:42:49 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180445 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/14/7211411.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_7211411
loop_
_publ_author_name
'Guo, Xiang-Guang'
'Yang, Wen-Bin'
'Wu, Xiao-Yuan'
'Zhang, Qi-Kai'
'Lu, Can-Zhong'
_publ_section_title
;
 Construction of coordination polymers based on
 methylenebis(3,5-dimethylpyrazole) and varied aromatic carboxylic acids
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              10107
_journal_paper_doi               10.1039/c3ce41575a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C16 H17 Cu N4 O4'
_chemical_formula_weight         392.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            16
_cell_length_a                   12.412(5)
_cell_length_b                   16.372(7)
_cell_length_c                   31.497(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6400(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            11957
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.8076
_exptl_absorpt_correction_T_min  0.7396
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1108P)²+3.2560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                1667
_reflns_number_total             1836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41575a.txt
_cod_data_source_block           a4
_cod_original_cell_volume        6401(4)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7211411
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.3750 0.3750 0.679761(12) 0.0164(2) Uani 1 2 d S
N2 N 0.59838(17) 0.44835(13) 0.67987(7) 0.0220(5) Uani 1 1 d .
H2D H 0.6199 0.4152 0.6605 0.026 Uiso 1 1 calc R
N1 N 0.50161(16) 0.44241(12) 0.70001(7) 0.0202(4) Uani 1 1 d .
C5 C 0.5945(2) 0.55112(14) 0.72485(7) 0.0187(5) Uani 1 1 d .
C4 C 0.49855(19) 0.50533(15) 0.72747(8) 0.0194(5) Uani 1 1 d .
C3 C 0.6560(2) 0.51200(15) 0.69391(8) 0.0217(5) Uani 1 1 d .
C2 C 0.4044(2) 0.51843(19) 0.75564(10) 0.0356(7) Uani 1 1 d .
H2A H 0.3512 0.4772 0.7502 0.053 Uiso 1 1 calc R
H2B H 0.3740 0.5713 0.7502 0.053 Uiso 1 1 calc R
H2C H 0.4269 0.5153 0.7847 0.053 Uiso 1 1 calc R
C1 C 0.7648(2) 0.53161(19) 0.67625(10) 0.0361(7) Uani 1 1 d .
H1A H 0.7839 0.4916 0.6553 0.054 Uiso 1 1 calc R
H1B H 0.8170 0.5310 0.6987 0.054 Uiso 1 1 calc R
H1C H 0.7632 0.5848 0.6634 0.054 Uiso 1 1 calc R
O2 O 0.45232(15) 0.27585(11) 0.66817(6) 0.0283(4) Uani 1 1 d .
O1 O 0.51303(15) 0.33532(10) 0.60955(6) 0.0282(4) Uani 1 1 d .
C9 C 0.56854(19) 0.19859(15) 0.62673(7) 0.0162(5) Uani 1 1 d .
C8 C 0.50769(18) 0.27704(14) 0.63415(8) 0.0177(5) Uani 1 1 d .
C7 C 0.5140(3) 0.1250 0.6250 0.0188(7) Uani 1 2 d S
H7A H 0.4391 0.1250 0.6250 0.023 Uiso 1 2 calc SR
C6 C 0.6250 0.6250 0.75043(12) 0.0255(8) Uani 1 2 d S
H6A H 0.681(3) 0.611(2) 0.7692(12) 0.046(10) Uiso 1 1 d .
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'
O O 0.0106 0.0060 '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
O2 Cu1 O2 158.09(12) 2 .
O2 Cu1 N1 89.26(8) 2 .
O2 Cu1 N1 97.63(8) . .
O2 Cu1 N1 97.63(8) 2 2
O2 Cu1 N1 89.26(8) . 2
N1 Cu1 N1 143.25(12) . 2
C3 N2 N1 111.9(2) . .
C4 N1 N2 105.64(19) . .
C4 N1 Cu1 126.74(16) . .
N2 N1 Cu1 125.25(16) . .
C3 C5 C4 105.0(2) . .
C3 C5 C6 127.4(2) . .
C4 C5 C6 127.6(2) . .
N1 C4 C5 110.2(2) . .
N1 C4 C2 121.2(2) . .
C5 C4 C2 128.6(2) . .
N2 C3 C5 107.2(2) . .
N2 C3 C1 121.8(2) . .
C5 C3 C1 131.0(2) . .
C8 O2 Cu1 114.63(15) . .
C7 C9 C9 119.01(16) . 11
C7 C9 C8 120.2(2) . .
C9 C9 C8 120.75(13) 11 .
O1 C8 O2 124.8(2) . .
O1 C8 C9 122.4(2) . .
O2 C8 C9 112.8(2) . .
C9 C7 C9 121.4(3) . 8_545
C5 C6 C5 115.1(3) . 14
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9208(18) 2
Cu1 O2 1.9208(18) .
Cu1 N1 2.024(2) .
Cu1 N1 2.024(2) 2
N2 C3 1.339(3) .
N2 N1 1.362(3) .
N1 C4 1.345(3) .
C5 C3 1.394(3) .
C5 C4 1.410(3) .
C5 C6 1.502(3) .
C4 C2 1.483(3) .
C3 C1 1.495(4) .
O2 C8 1.273(3) .
O1 C8 1.231(3) .
C9 C7 1.383(3) .
C9 C9 1.406(5) 11
C9 C8 1.508(3) .
C7 C9 1.383(3) 8_545
C6 C5 1.502(3) 14
