#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/44/2014430.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2014430
loop_
_publ_author_name
'Jaćimović, Željko K.'
'Leovac, Vukadin, M.'
'Mészáros Szécsényi, Katalin'
'Howard, Judith A. K.'
'Radosavljević Evans, Ivana'
_publ_section_title
;Transition metal complexes with pyrazole-based ligands. XIX.
 Diaquabis(3,5-dimethyl-1H-pyrazole-1-carboxamidine-κ²N,N')metal(II)
 dinitrate, with metal = Co and Ni
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m467
_journal_page_last               m470
_journal_paper_doi               10.1107/S0108270104017433
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C6 H10 N4)2 (H2 O)2] (N O3)2'
_chemical_formula_moiety         'C12 H24 Co N8 O2 2+ , 2N O3 -'
_chemical_formula_sum            'C12 H24 Co N10 O8'
_chemical_formula_weight         495.32
_chemical_name_systematic
;
Diaquabis(3,5-dimethylpyrazole-1-carboxamidine-κ²N,N')cobalt(II) dinitrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 107.602(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1067(11)
_cell_length_b                   10.9344(13)
_cell_length_c                   10.4425(13)
_cell_measurement_reflns_used    7486
_cell_measurement_temperature    120
_cell_measurement_theta_max      61.67
_cell_measurement_theta_min      5.21
_cell_volume                     991.1(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13055
_diffrn_reflns_theta_full        29.373
_diffrn_reflns_theta_max         30.919
_diffrn_reflns_theta_min         2.606
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.38
_refine_ls_goodness_of_fit_ref   0.9832
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.000628
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1982),
[weight] = 1/[A₀T₀(x)+A₁T₁(x) ... +Aₙ₋₁Tₙ₋₁(x)],
where Ai are the Chebychev coefficients listed below and x = Fcalc/Fₘₐₓ
Method = robust weighting (Prince, 1982),
W = [weight] × [1-(\DF/6\sF)²]².
Ai are 1.62, 2.12 and 0.556
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0620
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                2920
_reflns_number_total             2975
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bm1571.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2014430
_cod_database_fobs_code          2014430
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Co1 1.0000 0.5000 1.0000 0.0127 Uani 1.0000 . . Co
N1 1.20636(9) 0.29222(7) 1.00939(8) 0.0146 Uani 1.0000 . . N
N2 1.05102(8) 0.31803(7) 0.97054(8) 0.0151 Uani 1.0000 . . N
N3 1.23936(10) 0.49253(7) 1.07683(9) 0.0161 Uani 1.0000 . . N
N4 1.45759(10) 0.37046(9) 1.09871(9) 0.0204 Uani 1.0000 . . N
N5 1.33613(9) 0.34672(8) 0.74332(8) 0.0171 Uani 1.0000 . . N
C1 1.30604(10) 0.39099(9) 1.06510(9) 0.0151 Uani 1.0000 . . C
C2 0.80811(11) 0.20551(9) 0.87785(11) 0.0206 Uani 1.0000 . . C
C3 0.97959(10) 0.21337(8) 0.92762(9) 0.0157 Uani 1.0000 . . C
C4 1.08791(11) 0.11904(8) 0.93680(10) 0.0178 Uani 1.0000 . . C
C5 1.23080(11) 0.17100(8) 0.98816(9) 0.0165 Uani 1.0000 . . C
C6 1.38285(12) 0.11031(10) 1.01281(12) 0.0231 Uani 1.0000 . . C
O1 1.23276(9) 0.27136(8) 0.69350(9) 0.0309 Uani 1.0000 . . O
O2 1.30401(9) 0.45101(7) 0.77817(8) 0.0219 Uani 1.0000 . . O
O3 1.47423(9) 0.31926(8) 0.75900(9) 0.0275 Uani 1.0000 . . O
O4 1.02884(8) 0.55437(7) 0.80883(7) 0.0183 Uani 1.0000 . . O
H1 1.297(2) 0.5397(17) 1.1074(16) 0.027(4) Uiso 1.0000 . . H
H2 1.0670(17) 0.0377(15) 0.9125(14) 0.020(3) Uiso 1.0000 . . H
H3 0.7762(19) 0.1272(17) 0.8487(16) 0.035(4) Uiso 1.0000 . . H
H4 0.7637(18) 0.2253(16) 0.9478(15) 0.029(4) Uiso 1.0000 . . H
H5 0.765(2) 0.2578(16) 0.8001(17) 0.032(4) Uiso 1.0000 . . H
H6 1.362(2) 0.030(2) 0.9825(19) 0.041(5) Uiso 1.0000 . . H
H7 1.4387(19) 0.1133(16) 1.1032(16) 0.029(4) Uiso 1.0000 . . H
H8 1.4425(19) 0.1488(15) 0.9590(15) 0.027(4) Uiso 1.0000 . . H
H9 1.4919(19) 0.2992(18) 1.1012(16) 0.034(4) Uiso 1.0000 . . H
H10 1.514(2) 0.4268(17) 1.1324(16) 0.028(4) Uiso 1.0000 . . H
H11 1.103(2) 0.5260(18) 0.8003(18) 0.035(4) Uiso 1.0000 . . H
H12 1.037(2) 0.6309(19) 0.7992(18) 0.042(5) Uiso 1.0000 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.00943(9) 0.01169(9) 0.01636(9) 0.00113(5) 0.00285(6) -0.00073(5)
N1 0.0107(3) 0.0139(3) 0.0182(3) 0.0025(3) 0.0027(2) -0.0004(3)
N2 0.0092(3) 0.0150(3) 0.0201(3) 0.0017(3) 0.0030(3) -0.0015(3)
N3 0.0120(4) 0.0142(3) 0.0207(4) -0.0004(3) 0.0030(3) -0.0022(3)
N4 0.0109(3) 0.0188(4) 0.0287(4) 0.0027(3) 0.0018(3) -0.0028(3)
N5 0.0137(3) 0.0192(4) 0.0179(3) -0.0011(3) 0.0039(3) 0.0008(3)
C1 0.0125(4) 0.0167(4) 0.0153(4) 0.0000(3) 0.0029(3) -0.0003(3)
C2 0.0129(4) 0.0195(4) 0.0281(4) -0.0023(3) 0.0043(3) -0.0061(4)
C3 0.0140(4) 0.0148(4) 0.0182(4) -0.0001(3) 0.0048(3) -0.0010(3)
C4 0.0175(4) 0.0141(4) 0.0222(4) 0.0016(3) 0.0065(3) -0.0010(3)
C5 0.0160(4) 0.0146(4) 0.0188(4) 0.0036(3) 0.0052(3) 0.0006(3)
C6 0.0170(4) 0.0185(4) 0.0323(5) 0.0065(3) 0.0049(4) -0.0014(4)
O1 0.0190(4) 0.0276(4) 0.0434(5) -0.0085(3) 0.0052(3) -0.0082(4)
O2 0.0180(3) 0.0188(3) 0.0299(4) 0.0016(3) 0.0087(3) -0.0005(3)
O3 0.0131(3) 0.0275(4) 0.0416(4) 0.0013(3) 0.0078(3) -0.0087(3)
O4 0.0161(3) 0.0183(3) 0.0216(3) 0.0018(3) 0.0072(2) 0.0016(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C   ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0061 0.0033 International_Tables_Vol_IV_Table_2.2B
'O   ' 0.0106 0.0060 International_Tables_Vol_IV_Table_2.2B
'Co  ' 0.3494 0.9721 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N2 Co1 N3 76.46(3) yes
N2 Co1 O4 91.79(3) yes
N3 Co1 O4 87.79(3) yes
N2 N1 C1 115.97(7) no
N2 N1 C5 110.63(7) no
C1 N1 C5 133.37(8) no
Co1 N2 N1 113.98(6) no
Co1 N2 C3 139.86(6) no
N1 N2 C3 106.14(7) no
Co1 N3 C1 117.72(7) no
Co1 N3 H1 131.5(14) no
C1 N3 H1 110.7(14) no
O1 N5 O2 120.66(8) no
O1 N5 O3 119.95(9) no
O2 N5 O3 119.39(8) no
C1 N4 H9 120.7(12) no
C1 N4 H10 116.9(12) no
H9 N4 H10 120.9(16) no
N1 C1 N4 117.53(8) no
N1 C1 N3 115.70(8) no
N4 C1 N3 126.77(9) no
C3 C2 H3 111.1(10) no
C3 C2 H4 111.1(9) no
H3 C2 H4 107.2(14) no
C3 C2 H5 111.8(10) no
H3 C2 H5 105.2(14) no
H4 C2 H5 110.2(14) no
C2 C3 N2 121.50(8) no
C2 C3 C4 128.21(8) no
N2 C3 C4 110.29(8) no
C3 C4 C5 106.56(8) no
C3 C4 H2 126.9(9) no
C5 C4 H2 126.5(9) no
N1 C5 C4 106.38(8) no
N1 C5 C6 126.24(9) no
C4 C5 C6 127.36(9) no
C5 C6 H6 106.2(12) no
C5 C6 H7 110.9(10) no
H6 C6 H7 111.7(15) no
C5 C6 H8 110.8(9) no
H6 C6 H8 107.3(15) no
H7 C6 H8 109.8(14) no
Co1 O4 H11 110.4(14) no
Co1 O4 H12 114.7(12) no
H11 O4 H12 105.7(18) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N2 . . 2.0871(8) yes
Co1 N3 . . 2.0842(9) yes
Co1 O4 . . 2.1737(7) yes
N1 N2 . . 1.3778(10) yes
N1 C1 . . 1.4176(12) yes
N1 C5 . . 1.3731(12) yes
N2 C3 . . 1.3256(12) yes
N3 C1 . . 1.2890(12) yes
N3 H1 . . 0.734(19) no
N5 O1 . . 1.2408(11) yes
N5 O2 . . 1.2582(11) yes
N5 O3 . . 1.2546(11) yes
N4 C1 . . 1.3361(12) yes
N4 H9 . . 0.837(19) no
N4 H10 . . 0.809(18) no
C2 C3 . . 1.4918(13) yes
C2 H3 . . 0.926(18) no
C2 H4 . . 0.960(16) no
C2 H5 . . 0.973(17) no
C3 C4 . . 1.4104(12) yes
C4 C5 . . 1.3717(13) yes
C4 H2 . . 0.929(16) no
C5 C6 . . 1.4860(13) yes
C6 H6 . . 0.93(2) no
C6 H7 . . 0.927(16) no
C6 H8 . . 0.986(16) no
O4 H11 . . 0.78(2) no
O4 H12 . . 0.85(2) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N4 H9 O1 4_555 0.84(2) 2.249(18) 2.8572(13) 129.7(16)
N4 H10 O2 2_867 0.811(18) 2.114(18) 2.9136(13) 168.8(18)
O4 H11 O2 . 0.772(19) 2.081(19) 2.8539(12) 179.5(14)
O4 H12 O3 3_756 0.85(2) 2.14(2) 2.9799(12) 169.6(18)
