#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:02:04 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179552 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/21/4502136.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_4502136
loop_
_publ_author_name
'Lipstman, Sophia'
'Goldberg, Israel'
_publ_section_title
;
 Supramolecular Crystal Chemistry of Tetra(3-pyridyl)porphyrin. 2. Two-
 and Three-Dimensional Coordination Networks with Cobalt and Cadmium Ions
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5001
_journal_paper_doi               10.1021/cg1011007
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C40 H24 Br4 Cu5 N8'
_chemical_formula_sum            'C40 H24 Br4 Cu5 N8'
_chemical_formula_weight         1254.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            4
_cell_length_a                   15.0113(3)
_cell_length_b                   15.0113(3)
_cell_length_c                   17.3605(4)
_cell_measurement_reflns_used    2224
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      3.03
_cell_volume                     3912.00(14)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9214
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.803
_exptl_absorpt_correction_T_max  0.3432
_exptl_absorpt_correction_T_min  0.2811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.127
_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     129
_refine_ls_number_reflns         2321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0379
_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)+(0.0498P)²+1.7409P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                1854
_reflns_number_total             2321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1011007_si_001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4502136
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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 0.0000 -0.2500 0.3750 0.0183(2) Uani 1 4 d S
C1 C 0.2003(2) -0.2246(3) 0.3760(2) 0.0231(8) Uani 1 1 d .
C2 C 0.2680(3) -0.1561(3) 0.3727(2) 0.0285(9) Uani 1 1 d .
H2 H 0.3306 -0.1651 0.3723 0.034 Uiso 1 1 calc R
C3 C 0.2251(3) -0.0769(3) 0.3704(2) 0.0285(9) Uani 1 1 d .
H3 H 0.2521 -0.0197 0.3677 0.034 Uiso 1 1 calc R
C4 C 0.1314(2) -0.0954(2) 0.3728(2) 0.0222(7) Uani 1 1 d .
C5 C 0.0645(3) -0.0309(2) 0.3713(2) 0.0221(7) Uani 1 1 d .
N6 N 0.1170(2) -0.1864(2) 0.37600(17) 0.0204(6) Uani 1 1 d .
C7 C 0.0932(3) 0.0644(2) 0.3636(2) 0.0233(8) Uani 1 1 d .
C8 C 0.0959(3) 0.1022(3) 0.2906(2) 0.0304(9) Uani 1 1 d .
H8 H 0.0810 0.0661 0.2476 0.036 Uiso 1 1 calc R
N9 N 0.1188(2) 0.1877(2) 0.2782(2) 0.0310(8) Uani 1 1 d .
C10 C 0.1426(3) 0.2370(3) 0.3392(2) 0.0290(9) Uani 1 1 d .
H10 H 0.1613 0.2966 0.3308 0.035 Uiso 1 1 calc R
C11 C 0.1412(3) 0.2053(3) 0.4126(3) 0.0345(10) Uani 1 1 d .
H11 H 0.1573 0.2426 0.4546 0.041 Uiso 1 1 calc R
C12 C 0.1155(3) 0.1169(3) 0.4254(2) 0.0342(10) Uani 1 1 d .
H12 H 0.1135 0.0935 0.4762 0.041 Uiso 1 1 calc R
Cu2 Cu 0.10613(4) 0.23926(3) 0.17095(3) 0.03240(17) Uani 1 1 d .
Br Br 0.14669(3) 0.13937(3) 0.07197(2) 0.03228(15) Uani 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N6 Cu1 N6 179.00(17) . 2_545
N6 Cu1 N6 90.005(2) . 12_556
N6 Cu1 N6 90.004(2) 2_545 12_556
N6 Cu1 N6 90.004(2) . 11_656
N6 Cu1 N6 90.004(2) 2_545 11_656
N6 Cu1 N6 179.01(17) 12_556 11_656
N6 C1 C5 126.4(3) . 11_656
N6 C1 C2 110.0(3) . .
C5 C1 C2 123.6(4) 11_656 .
C3 C2 C1 107.0(3) . .
C3 C2 H2 126.5 . .
C1 C2 H2 126.5 . .
C2 C3 C4 107.1(3) . .
C2 C3 H3 126.4 . .
C4 C3 H3 126.4 . .
N6 C4 C5 125.0(3) . .
N6 C4 C3 110.2(3) . .
C5 C4 C3 124.7(4) . .
C1 C5 C4 124.1(4) 12_556 .
C1 C5 C7 118.6(3) 12_556 .
C4 C5 C7 117.3(3) . .
C1 N6 C4 105.6(3) . .
C1 N6 Cu1 126.9(2) . .
C4 N6 Cu1 127.5(2) . .
C12 C7 C8 118.1(4) . .
C12 C7 C5 123.3(4) . .
C8 C7 C5 118.7(3) . .
N9 C8 C7 123.0(4) . .
N9 C8 H8 118.5 . .
C7 C8 H8 118.5 . .
C10 N9 C8 117.8(3) . .
C10 N9 Cu2 122.7(3) . .
C8 N9 Cu2 119.3(3) . .
N9 C10 C11 122.9(4) . .
N9 C10 H10 118.6 . .
C11 C10 H10 118.6 . .
C10 C11 C12 118.9(4) . .
C10 C11 H11 120.5 . .
C12 C11 H11 120.5 . .
C7 C12 C11 119.2(4) . .
C7 C12 H12 120.4 . .
C11 C12 H12 120.4 . .
N9 Cu2 Br 113.70(10) . .
N9 Cu2 Br 109.35(10) . 16
Br Cu2 Br 131.65(2) . 16
N9 Cu2 Cu2 113.02(10) . 15
Br Cu2 Cu2 54.25(2) . 15
Br Cu2 Cu2 124.33(2) 16 15
N9 Cu2 Cu2 145.10(11) . 16
Br Cu2 Cu2 96.69(3) . 16
Br Cu2 Cu2 54.02(2) 16 16
Cu2 Cu2 Cu2 70.63(2) 15 16
Cu2 Br Cu2 71.73(3) . 15
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N6 1.998(3) .
Cu1 N6 1.998(3) 2_545
Cu1 N6 1.998(3) 12_556
Cu1 N6 1.998(3) 11_656
C1 N6 1.377(5) .
C1 C5 1.380(5) 11_656
C1 C2 1.446(5) .
C2 C3 1.353(6) .
C2 H2 0.9500 .
C3 C4 1.435(5) .
C3 H3 0.9500 .
C4 N6 1.384(5) .
C4 C5 1.395(5) .
C5 C1 1.380(5) 12_556
C5 C7 1.499(5) .
C7 C12 1.372(6) .
C7 C8 1.389(6) .
C8 N9 1.345(5) .
C8 H8 0.9500 .
N9 C10 1.341(5) .
N9 Cu2 2.025(3) .
C10 C11 1.361(6) .
C10 H10 0.9500 .
C11 C12 1.400(6) .
C11 H11 0.9500 .
C12 H12 0.9500 .
Cu2 Br 2.3604(7) .
Cu2 Br 2.3676(6) 16
Cu2 Cu2 2.7701(9) 15
Cu2 Cu2 2.7702(9) 16
Br Cu2 2.3675(6) 15
