#------------------------------------------------------------------------------
#$Date: 2015-09-23 09:17:04 +0300 (Wed, 23 Sep 2015) $
#$Revision: 158249 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/22/7222277.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_7222277
loop_
_publ_author_name
'Baruah, Jubaraj Bikash'
'Tarai, Arup'
_publ_section_title
;
 Study on divalent copper, nickel and zinc model complexes for fluoride
 ions detection
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA18559A
_journal_year                    2015
_chemical_formula_moiety         'C14 H12 N2 Ni O6, 2(C3 H7 N O)'
_chemical_formula_sum            'C20 H26 N4 Ni O8'
_chemical_formula_weight         509.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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
_audit_update_record
;
2015-06-22 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.288(5)
_cell_angle_beta                 101.143(5)
_cell_angle_gamma                100.988(5)
_cell_formula_units_Z            1
_cell_length_a                   6.2331(6)
_cell_length_b                   7.2148(6)
_cell_length_c                   13.1150(12)
_cell_measurement_temperature    296(2)
_cell_volume                     567.52(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6679
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-Scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Neddle
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2044
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.600
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0738
_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)+(0.0000P)²+7.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                1883
_reflns_number_total             2044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra18559a2.cif
_cod_data_source_block           Complex-5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               7222277
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
C3 C 0.2803(9) -0.1238(8) 0.3739(5) 0.033(2) Uani 1 1 d G
C2 C 0.4044(11) 0.0570(7) 0.3703(5) 0.032(2) Uani 1 1 d G
C7 C 0.5824(11) 0.0852(7) 0.3188(6) 0.041(3) Uani 1 1 d G
H7 H 0.6655 0.2061 0.3164 0.050 Uiso 1 1 calc R
C6 C 0.6362(10) -0.0673(9) 0.2710(6) 0.043(3) Uani 1 1 d G
H6 H 0.7553 -0.0485 0.2366 0.052 Uiso 1 1 calc R
C5 C 0.5121(12) -0.2481(8) 0.2747(5) 0.039(2) Uani 1 1 d GD
C4 C 0.3341(11) -0.2763(7) 0.3261(5) 0.038(2) Uani 1 1 d G
H4 H 0.2510 -0.3973 0.3286 0.045 Uiso 1 1 calc R
Ni1 Ni 0.0000 0.0000 0.5000 0.0290(5) Uani 1 2 d S
O2 O 0.1816(14) 0.3906(10) 0.5060(7) 0.048(2) Uani 1 1 d .
H2 H 0.0779 0.3812 0.5370 0.072 Uiso 1 1 calc R
O3 O 0.5592(16) -0.4052(12) 0.2290(7) 0.059(2) Uani 1 1 d D
H3 H 0.6666 -0.3727 0.2011 0.089 Uiso 1 1 calc R
O1 O 0.1124(12) -0.1564(9) 0.4255(6) 0.0390(18) Uani 1 1 d D
N1 N 0.1933(14) 0.2052(11) 0.4668(7) 0.0333(19) Uani 1 1 d D
C1 C 0.3565(18) 0.2213(14) 0.4187(8) 0.036(2) Uani 1 1 d .
H1A H 0.4447 0.3396 0.4149 0.043 Uiso 1 1 calc R
O4 O 1.209(3) 0.306(2) -0.0795(11) 0.108(5) Uani 1 1 d .
N2 N 0.9750(19) 0.2492(15) 0.0301(9) 0.054(3) Uani 1 1 d .
C9 C 1.113(3) 0.253(3) 0.1287(15) 0.107(7) Uani 1 1 d .
H9A H 1.1096 0.1267 0.1514 0.161 Uiso 1 1 calc R
H9B H 1.0615 0.3254 0.1773 0.161 Uiso 1 1 calc R
H9C H 1.2635 0.3109 0.1247 0.161 Uiso 1 1 calc R
C8 C 0.736(3) 0.203(3) 0.0233(19) 0.115(8) Uani 1 1 d .
H8A H 0.6615 0.2344 -0.0435 0.172 Uiso 1 1 calc R
H8B H 0.6961 0.2729 0.0768 0.172 Uiso 1 1 calc R
H8C H 0.6912 0.0698 0.0323 0.172 Uiso 1 1 calc R
C10 C 1.052(5) 0.280(3) -0.057(2) 0.133(11) Uani 1 1 d .
H10 H 0.9367 0.2774 -0.1139 0.160 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'
Ni Ni 0.3393 1.1124 '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'
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
O1 C3 C2 121.4(5) . .
O1 C3 C4 118.6(5) . .
C2 C3 C4 120.0 . .
C3 C2 C7 120.0 . .
C3 C2 C1 122.5(6) . .
C7 C2 C1 117.5(6) . .
C2 C7 C6 120.0 . .
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C5 C6 C7 120.0 . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
O3 C5 C6 122.4(6) . .
O3 C5 C4 117.6(6) . .
C6 C5 C4 120.0 . .
C5 C4 C3 120.0 . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
O1 Ni1 O1 179.999(2) 2_556 .
O1 Ni1 N1 90.8(3) 2_556 2_556
O1 Ni1 N1 89.2(3) . 2_556
O1 Ni1 N1 89.2(3) 2_556 .
O1 Ni1 N1 90.8(3) . .
N1 Ni1 N1 179.999(1) 2_556 .
N1 O2 H2 109.5 . .
C5 O3 H3 109.5 . .
C3 O1 Ni1 131.7(5) . .
C1 N1 O2 109.0(8) . .
C1 N1 Ni1 132.6(7) . .
O2 N1 Ni1 118.2(6) . .
N1 C1 C2 120.6(9) . .
N1 C1 H1A 119.7 . .
C2 C1 H1A 119.7 . .
C10 N2 C9 123.4(19) . .
C10 N2 C8 119(2) . .
C9 N2 C8 118.0(15) . .
N2 C9 H9A 109.5 . .
N2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O4 C10 N2 138(3) . .
O4 C10 H10 111.2 . .
N2 C10 H10 111.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3 O1 1.337(8) .
C3 C2 1.3900 .
C3 C4 1.3900 .
C2 C7 1.3900 .
C2 C1 1.448(11) .
C7 C6 1.3900 .
C7 H7 0.9300 .
C6 C5 1.3900 .
C6 H6 0.9300 .
C5 O3 1.385(8) .
C5 C4 1.3900 .
C4 H4 0.9300 .
Ni1 O1 1.809(7) 2_556
Ni1 O1 1.809(7) .
Ni1 N1 1.834(8) 2_556
Ni1 N1 1.834(8) .
O2 N1 1.451(10) .
O2 H2 0.8200 .
O3 H3 0.8200 .
N1 C1 1.285(13) .
C1 H1A 0.9300 .
O4 C10 1.06(3) .
N2 C10 1.32(2) .
N2 C9 1.406(19) .
N2 C8 1.45(2) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C10 H10 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O1 C3 C2 C7 178.0(7) .
C4 C3 C2 C7 0.0 .
O1 C3 C2 C1 -2.0(9) .
C4 C3 C2 C1 -179.9(8) .
C3 C2 C7 C6 0.0 .
C1 C2 C7 C6 179.9(7) .
C2 C7 C6 C5 0.0 .
C7 C6 C5 O3 -179.6(8) .
C7 C6 C5 C4 0.0 .
O3 C5 C4 C3 179.6(8) .
C6 C5 C4 C3 0.0 .
O1 C3 C4 C5 -178.0(7) .
C2 C3 C4 C5 0.0 .
C2 C3 O1 Ni1 -0.3(11) .
C4 C3 O1 Ni1 177.6(5) .
O1 Ni1 O1 C3 78(6) 2_556
N1 Ni1 O1 C3 -176.6(8) 2_556
N1 Ni1 O1 C3 3.4(8) .
O1 Ni1 N1 C1 173.7(11) 2_556
O1 Ni1 N1 C1 -6.3(11) .
N1 Ni1 N1 C1 -158(20) 2_556
O1 Ni1 N1 O2 -1.0(7) 2_556
O1 Ni1 N1 O2 179.0(7) .
N1 Ni1 N1 O2 28(20) 2_556
O2 N1 C1 C2 -179.2(8) .
Ni1 N1 C1 C2 5.8(16) .
C3 C2 C1 N1 -0.6(13) .
C7 C2 C1 N1 179.5(8) .
C9 N2 C10 O4 3(4) .
C8 N2 C10 O4 -175(3) .
