#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:41:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179731 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002733.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_7002733
loop_
_publ_author_name
'Rodríguez-Diéguez, Antonio'
'Mota, Antonio J.'
'Seco, José M.'
'Palacios, María A.'
'Romerosa, Antonio'
'Colacio, Enrique'
_publ_section_title
;
 Influence of metal ions, coligands and reaction conditions on the
 structural versatility and properties of 5-pyrimidyl-tetrazolate
 containing complexes
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              9578
_journal_page_last               9586
_journal_paper_doi               10.1039/b910811d
_journal_year                    2009
_chemical_formula_sum            'C11 H21 Cl Cu N10 O4'
_chemical_formula_weight         456.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.5550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2828(5)
_cell_length_b                   7.8531(3)
_cell_length_c                   15.2177(5)
_cell_measurement_reflns_used    2743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.41
_cell_volume                     1731.45(10)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9209
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blu
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0293
_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/[σ²(Fo²)+(0.0444P)²+0.4293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2743
_reflns_number_total             3054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910811d.txt
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7002733
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.762256(17) 0.22072(3) 0.393581(18) 0.01164(11) Uani 1 1 d . . .
Cl1 Cl 0.38430(4) 0.23288(7) 0.02406(4) 0.01527(15) Uani 1 1 d . . .
O1 O 0.35313(12) 0.2344(2) 0.10412(13) 0.0262(4) Uani 1 1 d . . .
O2 O 0.33815(13) 0.3637(2) -0.03917(12) 0.0319(5) Uani 1 1 d . . .
O3 O 0.36269(13) 0.0708(2) -0.02154(12) 0.0312(4) Uani 1 1 d . . .
O4 O 0.48173(12) 0.2619(3) 0.05370(13) 0.0337(5) Uani 1 1 d . . .
N1A N 1.08475(12) 0.3488(2) 0.51579(13) 0.0155(4) Uani 1 1 d . . .
N2A N 0.98478(12) 0.1461(2) 0.41515(12) 0.0139(4) Uani 1 1 d . . .
N3A N 0.98107(14) 0.2700(2) 0.64073(14) 0.0160(4) Uani 1 1 d . . .
N4A N 0.90460(14) 0.2587(2) 0.66676(14) 0.0177(5) Uani 1 1 d . . .
N5A N 0.83169(14) 0.2329(2) 0.59398(14) 0.0172(4) Uani 1 1 d . . .
N6A N 0.85878(13) 0.2252(2) 0.51800(13) 0.0135(4) Uani 1 1 d . . .
N1B N 0.65568(13) 0.2328(2) 0.27021(13) 0.0119(4) Uani 1 1 d . . .
N2B N 0.82410(12) 0.3943(2) 0.32988(12) 0.0136(4) Uani 1 1 d . . .
H2B1 H 0.8594 0.4678 0.3717 0.016 Uiso 1 1 calc R . .
H2B2 H 0.8598 0.3406 0.3016 0.016 Uiso 1 1 calc R . .
N3B N 0.78516(12) -0.0270(2) 0.34490(13) 0.0159(4) Uani 1 1 d . . .
H3B1 H 0.8457 -0.0437 0.3540 0.019 Uiso 1 1 calc R . .
H3B2 H 0.7648 -0.1089 0.3750 0.019 Uiso 1 1 calc R . .
N4B N 0.65810(13) 0.2168(2) 0.45154(14) 0.0170(4) Uani 1 1 d . . .
H4B1 H 0.6654 0.1262 0.4894 0.020 Uiso 1 1 calc R . .
H4B2 H 0.6611 0.3115 0.4857 0.020 Uiso 1 1 calc R . .
C1A C 1.03833(15) 0.1503(3) 0.36065(15) 0.0163(5) Uani 1 1 d . . .
H1A H 1.0234 0.0814 0.3082 0.020 Uiso 1 1 calc R . .
C2A C 1.11488(17) 0.2535(3) 0.37984(18) 0.0196(5) Uani 1 1 d . . .
H2A H 1.1506 0.2582 0.3406 0.023 Uiso 1 1 calc R . .
C3A C 1.13641(15) 0.3497(3) 0.45958(16) 0.0189(5) Uani 1 1 d . . .
H3A H 1.1889 0.4178 0.4749 0.023 Uiso 1 1 calc R . .
C4A C 1.01028(16) 0.2472(3) 0.48979(16) 0.0129(5) Uani 1 1 d . . .
C5A C 0.95089(16) 0.2479(3) 0.54886(16) 0.0130(5) Uani 1 1 d . . .
C1B C 0.56652(15) 0.2075(3) 0.37911(16) 0.0180(5) Uani 1 1 d . . .
H1B1 H 0.5204 0.2631 0.4006 0.022 Uiso 1 1 calc R . .
H1B2 H 0.5485 0.0895 0.3655 0.022 Uiso 1 1 calc R . .
C2B C 0.74775(15) 0.4846(3) 0.26158(15) 0.0155(5) Uani 1 1 d . . .
H2B3 H 0.7713 0.5520 0.2206 0.019 Uiso 1 1 calc R . .
H2B4 H 0.7173 0.5604 0.2930 0.019 Uiso 1 1 calc R . .
C3B C 0.73277(15) -0.0295(3) 0.24517(15) 0.0162(5) Uani 1 1 d . . .
H3B3 H 0.7230 -0.1461 0.2232 0.019 Uiso 1 1 calc R . .
H3B4 H 0.7670 0.0296 0.2106 0.019 Uiso 1 1 calc R . .
C4B C 0.64077(15) 0.0574(3) 0.23076(15) 0.0149(5) Uani 1 1 d . . .
H4B3 H 0.6069 0.0630 0.1650 0.018 Uiso 1 1 calc R . .
H4B4 H 0.6045 -0.0080 0.2608 0.018 Uiso 1 1 calc R . .
C5B C 0.57318(15) 0.2953(3) 0.29294(16) 0.0159(5) Uani 1 1 d . . .
H5B1 H 0.5178 0.2727 0.2414 0.019 Uiso 1 1 calc R . .
H5B2 H 0.5779 0.4174 0.3030 0.019 Uiso 1 1 calc R . .
C6B C 0.68016(15) 0.3527(3) 0.20640(15) 0.0142(5) Uani 1 1 d . . .
H6B1 H 0.6249 0.4088 0.1674 0.017 Uiso 1 1 calc R . .
H6B2 H 0.7075 0.2905 0.1667 0.017 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N6A Cu1 N4B 91.88(8) . . ?
N6A Cu1 N1B 174.47(7) . . ?
N4B Cu1 N1B 84.02(7) . . ?
N6A Cu1 N2B 97.07(7) . . ?
N4B Cu1 N2B 138.13(8) . . ?
N1B Cu1 N2B 83.63(7) . . ?
N6A Cu1 N3B 100.98(7) . . ?
N4B Cu1 N3B 111.62(7) . . ?
N1B Cu1 N3B 84.01(7) . . ?
N2B Cu1 N3B 106.64(7) . . ?
O4 Cl1 O2 109.79(12) . . ?
O4 Cl1 O3 110.47(12) . . ?
O2 Cl1 O3 108.84(11) . . ?
O4 Cl1 O1 108.83(11) . . ?
O2 Cl1 O1 109.72(11) . . ?
O3 Cl1 O1 109.17(11) . . ?
C3A N1A C4A 115.6(2) . . ?
C1A N2A C4A 116.17(19) . . ?
C5A N3A N4A 104.79(18) . . ?
N5A N4A N3A 110.12(19) . . ?
N4A N5A N6A 108.70(18) . . ?
C5A N6A N5A 105.50(18) . . ?
C5A N6A Cu1 135.08(16) . . ?
N5A N6A Cu1 118.58(14) . . ?
C6B N1B C4B 111.16(17) . . ?
C6B N1B C5B 110.50(17) . . ?
C4B N1B C5B 111.41(17) . . ?
C6B N1B Cu1 109.57(13) . . ?
C4B N1B Cu1 107.45(13) . . ?
C5B N1B Cu1 106.57(13) . . ?
C2B N2B Cu1 105.68(13) . . ?
C3B N3B Cu1 105.82(13) . . ?
C1B N4B Cu1 111.06(14) . . ?
N2A C1A C2A 122.0(2) . . ?
C1A C2A C3A 117.3(2) . . ?
N1A C3A C2A 122.5(2) . . ?
N2A C4A N1A 126.4(2) . . ?
N2A C4A C5A 116.91(19) . . ?
N1A C4A C5A 116.7(2) . . ?
N3A C5A N6A 110.9(2) . . ?
N3A C5A C4A 124.5(2) . . ?
N6A C5A C4A 124.6(2) . . ?
N4B C1B C5B 108.28(18) . . ?
N2B C2B C6B 108.05(18) . . ?
N3B C3B C4B 108.55(17) . . ?
N1B C4B C3B 110.00(17) . . ?
N1B C5B C1B 110.21(18) . . ?
N1B C6B C2B 109.92(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N6A 1.9962(19) . ?
Cu1 N4B 2.0509(19) . ?
Cu1 N1B 2.0592(19) . ?
Cu1 N2B 2.0677(18) . ?
Cu1 N3B 2.1493(19) . ?
Cl1 O4 1.4301(19) . ?
Cl1 O2 1.4307(17) . ?
Cl1 O3 1.4369(18) . ?
Cl1 O1 1.4425(18) . ?
N1A C3A 1.336(3) . ?
N1A C4A 1.342(3) . ?
N2A C1A 1.338(3) . ?
N2A C4A 1.338(3) . ?
N3A C5A 1.337(3) . ?
N3A N4A 1.351(3) . ?
N4A N5A 1.313(3) . ?
N5A N6A 1.348(3) . ?
N6A C5A 1.346(3) . ?
N1B C6B 1.484(3) . ?
N1B C4B 1.491(3) . ?
N1B C5B 1.493(3) . ?
N2B C2B 1.474(3) . ?
N3B C3B 1.474(3) . ?
N4B C1B 1.482(3) . ?
C1A C2A 1.376(3) . ?
C2A C3A 1.377(3) . ?
C4A C5A 1.467(3) . ?
C1B C5B 1.514(3) . ?
C2B C6B 1.514(3) . ?
C3B C4B 1.515(3) . ?
