#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:41:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179731 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002732.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_7002732
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            'C9 H23 Cl N10 Ni O2'
_chemical_formula_weight         397.53
_chemical_name_systematic
;
?
;
_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                94.7760(10)
_cell_angle_beta                 108.3050(10)
_cell_angle_gamma                105.4280(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5313(6)
_cell_length_b                   8.8434(6)
_cell_length_c                   12.5234(8)
_cell_measurement_reflns_used    6120
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28240
_cell_measurement_theta_min      2430
_cell_volume                     850.22(10)
_computing_cell_refinement       'Bruker smart'
_computing_data_collection       'Bruker smart'
_computing_data_reduction        'Bruker smart'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8383
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.832676
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Empirical
_exptl_crystal_colour            PINK
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0319P)²+0.1899P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                2820
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910811d.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002732
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N1 N 0.26944(16) 0.02777(15) 0.10476(11) 0.0334(3) Uani 1 1 d . . .
N2 N 0.13764(18) -0.10824(17) 0.07416(12) 0.0397(3) Uani 1 1 d . . .
C5 C 0.3021(2) 0.05293(19) 0.00948(13) 0.0336(3) Uani 1 1 d . . .
C6 C 0.4421(2) 0.19411(19) 0.01350(13) 0.0336(3) Uani 1 1 d . . .
N11 N 0.4784(2) 0.21653(18) -0.08094(12) 0.0432(4) Uani 1 1 d . . .
N4 N 0.19791(19) -0.06168(17) -0.07967(12) 0.0423(3) Uani 1 1 d . . .
N3 N 0.09542(19) -0.16112(18) -0.03619(13) 0.0450(4) Uani 1 1 d . . .
C8 C 0.6570(2) 0.4160(2) 0.12496(15) 0.0407(4) Uani 1 1 d . . .
H6A H 0.7174 0.4848 0.1950 0.049 Uiso 1 1 calc R . .
C9 C 0.7060(3) 0.4482(2) 0.03268(16) 0.0466(4) Uani 1 1 d . . .
H5A H 0.7989 0.5365 0.0391 0.056 Uiso 1 1 calc R . .
C10 C 0.6125(3) 0.3449(2) -0.06912(16) 0.0476(4) Uani 1 1 d . . .
H4A H 0.6434 0.3647 -0.1327 0.057 Uiso 1 1 calc R . .
C2B C 0.7476(2) 0.1448(2) 0.40380(15) 0.0424(4) Uani 1 1 d . . .
H1B2 H 0.8515 0.1132 0.4160 0.051 Uiso 1 1 calc R . .
H2B2 H 0.6962 0.1070 0.4594 0.051 Uiso 1 1 calc R . .
C3C C 0.1520(2) 0.1162(2) 0.33691(17) 0.0478(4) Uani 1 1 d . . .
H1C3 H 0.1094 0.0941 0.3990 0.057 Uiso 1 1 calc R . .
H2C3 H 0.0667 0.0482 0.2667 0.057 Uiso 1 1 calc R . .
C3B C 0.7937(2) 0.3242(2) 0.41894(16) 0.0452(4) Uani 1 1 d . . .
H2B3 H 0.8663 0.3718 0.4976 0.054 Uiso 1 1 calc R . .
H1B3 H 0.8580 0.3631 0.3700 0.054 Uiso 1 1 calc R . .
C2C C 0.1794(3) 0.2890(2) 0.32635(17) 0.0504(5) Uani 1 1 d . . .
H2C2 H 0.0690 0.3106 0.3049 0.061 Uiso 1 1 calc R . .
H1C2 H 0.2546 0.3567 0.3993 0.061 Uiso 1 1 calc R . .
N4C N 0.31819(19) 0.08332(19) 0.35936(13) 0.0364(3) Uani 1 1 d . . .
O1W O 0.0447(3) -0.2898(2) 0.24009(18) 0.0739(5) Uani 1 1 d D . .
O2W O 0.8325(3) 0.7182(2) 0.37523(18) 0.0769(5) Uani 1 1 d . . .
H21W H 0.877(4) 0.738(3) 0.329(2) 0.080(10) Uiso 1 1 d . . .
H11W H 0.066(4) -0.241(4) 0.179(2) 0.125(12) Uiso 1 1 d D . .
H12W H 0.129(4) -0.303(4) 0.274(3) 0.098(12) Uiso 1 1 d . . .
H22W H 0.752(4) 0.759(4) 0.353(3) 0.113(13) Uiso 1 1 d . . .
H1B1 H 0.578(2) -0.020(2) 0.2847(16) 0.036(5) Uiso 1 1 d . . .
H2B4 H 0.657(2) 0.471(2) 0.3788(16) 0.042(5) Uiso 1 1 d . . .
H1B4 H 0.603(2) 0.369(2) 0.4490(18) 0.043(5) Uiso 1 1 d . . .
H2B1 H 0.676(3) 0.078(2) 0.2433(18) 0.045(6) Uiso 1 1 d . . .
H1C4 H 0.380(2) 0.118(2) 0.4272(18) 0.037(5) Uiso 1 1 d . . .
H1C1 H 0.308(3) 0.424(2) 0.2488(16) 0.041(5) Uiso 1 1 d . . .
H2C1 H 0.180(3) 0.297(2) 0.1727(18) 0.048(6) Uiso 1 1 d . . .
H2C4 H 0.303(3) -0.020(3) 0.3477(18) 0.053(6) Uiso 1 1 d . . .
Ni1 Ni 0.43774(2) 0.19629(2) 0.251702(15) 0.02863(8) Uani 1 1 d . . .
Cl2 Cl 0.55703(6) 0.28117(5) -0.36836(4) 0.04517(12) Uani 1 1 d . . .
N4B N 0.63381(18) 0.36971(17) 0.38915(12) 0.0352(3) Uani 1 1 d . . .
N1C N 0.2588(2) 0.32426(19) 0.23884(13) 0.0364(3) Uani 1 1 d . . .
N7 N 0.52471(17) 0.28857(16) 0.11695(11) 0.0334(3) Uani 1 1 d . . .
N1B N 0.6235(2) 0.0740(2) 0.28706(13) 0.0379(3) 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'
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'
Ni Ni 0.3393 1.1124 '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
C5 N1 N2 105.25(12) . . ?
C5 N1 Ni1 114.70(10) . . ?
N2 N1 Ni1 139.95(11) . . ?
N3 N2 N1 108.35(14) . . ?
N1 C5 N4 112.26(15) . . ?
N1 C5 C6 119.28(13) . . ?
N4 C5 C6 128.46(15) . . ?
N11 C6 N7 126.26(16) . . ?
N11 C6 C5 119.26(14) . . ?
N7 C6 C5 114.46(14) . . ?
C6 N11 C10 115.61(15) . . ?
C5 N4 N3 103.81(14) . . ?
N2 N3 N4 110.34(13) . . ?
N7 C8 C9 121.83(16) . . ?
C10 C9 C8 117.26(17) . . ?
N11 C10 C9 122.76(17) . . ?
N1B C2B C3B 109.09(14) . . ?
N4C C3C C2C 108.70(15) . . ?
N4B C3B C2B 109.35(14) . . ?
N1C C2C C3C 109.36(14) . . ?
C3C N4C Ni1 107.63(11) . . ?
N4C Ni1 N1 93.66(6) . . ?
N4C Ni1 N1B 92.37(7) . . ?
N1 Ni1 N1B 93.36(5) . . ?
N4C Ni1 N1C 82.65(6) . . ?
N1 Ni1 N1C 92.24(6) . . ?
N1B Ni1 N1C 172.74(6) . . ?
N4C Ni1 N4B 93.13(6) . . ?
N1 Ni1 N4B 172.09(5) . . ?
N1B Ni1 N4B 82.29(6) . . ?
N1C Ni1 N4B 92.66(6) . . ?
N4C Ni1 N7 170.62(5) . . ?
N1 Ni1 N7 77.22(5) . . ?
N1B Ni1 N7 90.37(6) . . ?
N1C Ni1 N7 95.38(5) . . ?
N4B Ni1 N7 96.13(6) . . ?
C3B N4B Ni1 108.83(10) . . ?
C2C N1C Ni1 108.16(11) . . ?
C8 N7 C6 116.26(14) . . ?
C8 N7 Ni1 129.29(11) . . ?
C6 N7 Ni1 114.13(11) . . ?
C2B N1B Ni1 107.30(11) . . ?
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
N1 C5 1.331(2) . ?
N1 N2 1.3383(19) . ?
N1 Ni1 2.1010(12) . ?
N2 N3 1.322(2) . ?
C5 N4 1.331(2) . ?
C5 C6 1.465(2) . ?
C6 N11 1.331(2) . ?
C6 N7 1.344(2) . ?
N11 C10 1.339(2) . ?
N4 N3 1.343(2) . ?
C8 N7 1.337(2) . ?
C8 C9 1.374(3) . ?
C9 C10 1.370(3) . ?
C2B N1B 1.474(2) . ?
C2B C3B 1.510(3) . ?
C3C N4C 1.468(2) . ?
C3C C2C 1.507(3) . ?
C3B N4B 1.469(2) . ?
C2C N1C 1.473(2) . ?
N4C Ni1 2.0981(14) . ?
Ni1 N1B 2.1043(15) . ?
Ni1 N1C 2.1051(14) . ?
Ni1 N4B 2.1213(14) . ?
Ni1 N7 2.1812(13) . ?
