#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:30:10 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243950 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702684.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_7702684
loop_
_publ_author_name
'Murugavel, Ramaswamy'
'Krishnamurthy, Divya'
'Sathiyendiran, Malaichamy'
_publ_section_title
;
 Anionic metal--organic and cationic organic layer alternation in the
 coordination polymers [{M(BTEC)(OH2)4}·{C4H12N2}·4H2O]n (M
 = Co, Ni, and Zn; BTEC = 1,2,4,5-benzenetetracarboxylate)
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              34
_journal_paper_doi               10.1039/b105687p
_journal_year                    2002
_chemical_formula_moiety         '[Ni(H2O)4(C6H2(COO)4)]2-(C4H12N)2+(H2O)2'
_chemical_formula_sum            'C14 H30 N2 Ni O16'
_chemical_formula_weight         541.11
_chemical_name_common            'Ni_pyromelttate polymer'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                105.346(6)
_cell_angle_beta                 97.746(5)
_cell_angle_gamma                109.346(7)
_cell_formula_units_Z            1
_cell_length_a                   6.8436(4)
_cell_length_b                   9.1166(7)
_cell_length_c                   9.7167(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     534.86(7)
_computing_cell_refinement       'MACH3 Nonius software'
_computing_data_collection       'MACH3 Nonius software'
_computing_data_reduction        OSCAIL
_computing_molecular_graphics    PLATON99
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0038
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2059
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.6367
_exptl_absorpt_correction_T_min  0.5873
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangluar blocks'
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0314
_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)+(0.0493P)²+0.5261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                1863
_reflns_number_total             1882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105687p.txt
_cod_data_source_block           rm001
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        534.86(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702684
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_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.0000 0.0000 0.0000 0.01547(14) Uani 1 d S
O1 O 0.2532(3) 0.1662(2) -0.04415(18) 0.0243(3) Uani 1 d .
O2 O 0.1993(2) -0.0961(2) 0.08667(18) 0.0218(3) Uani 1 d .
O3 O 0.0284(2) 0.16030(17) 0.20953(15) 0.0193(3) Uani 1 d .
O4 O 0.2733(4) 0.3947(2) 0.2146(3) 0.0826(11) Uani 1 d .
O5 O -0.3472(2) 0.25221(19) 0.13085(16) 0.0245(4) Uani 1 d .
O6 O -0.4653(3) 0.1265(2) 0.28888(18) 0.0336(4) Uani 1 d .
O7 O 0.4079(4) -0.2697(3) 0.2641(3) 0.0502(6) Uani 1 d .
O8 O -0.1420(15) -0.4536(5) 0.0781(6) 0.168(4) Uani 1 d .
N1 N -0.1719(3) -0.0506(3) 0.3719(2) 0.0281(4) Uani 1 d .
C1 C 0.2124(3) 0.5401(3) 0.4987(2) 0.0205(4) Uani 1 d .
C2 C 0.0571(3) 0.4107(2) 0.3818(2) 0.0186(4) Uani 1 d .
C3 C -0.1588(3) 0.3713(2) 0.3828(2) 0.0182(4) Uani 1 d .
C4 C 0.1263(4) 0.3160(3) 0.2587(3) 0.0259(5) Uani 1 d .
C5 C -0.3379(3) 0.2381(3) 0.2568(2) 0.0203(4) Uani 1 d .
C6 C -0.0327(5) -0.1458(3) 0.3802(3) 0.0335(6) Uani 1 d .
C7 C -0.1858(4) 0.0353(4) 0.5218(3) 0.0323(5) Uani 1 d .
H1 H 0.374(7) 0.175(5) 0.007(5) 0.080 Uiso 1 d .
H2 H 0.247(7) 0.248(6) -0.028(5) 0.080 Uiso 1 d .
H3 H 0.234(7) -0.139(6) 0.023(5) 0.080 Uiso 1 d .
H4 H 0.292(7) -0.026(6) 0.150(5) 0.080 Uiso 1 d .
H5 H 0.361(7) 0.571(5) 0.502(5) 0.080 Uiso 1 d .
H6 H -0.122(7) 0.019(6) 0.323(5) 0.080 Uiso 1 d .
H7 H -0.309(7) -0.126(6) 0.318(5) 0.080 Uiso 1 d .
H8 H -0.022(7) -0.191(5) 0.283(5) 0.080 Uiso 1 d .
H9 H -0.099(7) -0.229(6) 0.417(5) 0.080 Uiso 1 d .
H10 H -0.271(7) 0.093(5) 0.508(5) 0.080 Uiso 1 d .
H11 H -0.255(7) -0.045(6) 0.565(5) 0.080 Uiso 1 d .
H12 H 0.408(7) -0.362(6) 0.246(5) 0.080 Uiso 1 d .
H13 H 0.316(7) -0.269(5) 0.194(5) 0.080 Uiso 1 d .
H14 H -0.107(9) -0.508(7) 0.092(7) 0.080 Uiso 1 d .
H15 H -0.284(8) -0.492(7) 0.078(6) 0.080 Uiso 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'
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
O2 Ni1 O2 180.00(9) . 2
O2 Ni1 O1 89.17(7) . 2
O2 Ni1 O1 90.83(7) 2 2
O2 Ni1 O1 90.83(7) . .
O2 Ni1 O1 89.17(7) 2 .
O1 Ni1 O1 180.00(8) 2 .
O2 Ni1 O3 92.05(6) . .
O2 Ni1 O3 87.95(6) 2 .
O1 Ni1 O3 85.10(6) 2 .
O1 Ni1 O3 94.90(6) . .
O2 Ni1 O3 87.95(6) . 2
O2 Ni1 O3 92.05(6) 2 2
O1 Ni1 O3 94.90(6) 2 2
O1 Ni1 O3 85.10(6) . 2
O3 Ni1 O3 180.00(9) . 2
C4 O3 Ni1 127.03(14) . .
C7 N1 C6 110.92(19) . .
C3 C1 C2 121.7(2) 2_566 .
C1 C2 C3 119.06(19) . .
C1 C2 C4 119.07(19) . .
C3 C2 C4 121.87(19) . .
C1 C3 C2 119.24(19) 2_566 .
C1 C3 C5 118.32(19) 2_566 .
C2 C3 C5 122.41(19) . .
O4 C4 O3 125.1(2) . .
O4 C4 C2 117.7(2) . .
O3 C4 C2 117.13(19) . .
O6 C5 O5 126.09(19) . .
O6 C5 C3 116.36(19) . .
O5 C5 C3 117.52(19) . .
N1 C6 C7 110.7(2) . 2_556
N1 C7 C6 111.1(2) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.0522(15) .
Ni1 O2 2.0522(15) 2
Ni1 O1 2.0707(16) 2
Ni1 O1 2.0707(16) .
Ni1 O3 2.1091(14) .
Ni1 O3 2.1091(14) 2
O3 C4 1.271(3) .
O4 C4 1.229(3) .
O5 C5 1.260(3) .
O6 C5 1.243(3) .
N1 C7 1.492(3) .
N1 C6 1.493(3) .
C1 C3 1.389(3) 2_566
C1 C2 1.395(3) .
C2 C3 1.402(3) .
C2 C4 1.510(3) .
C3 C1 1.389(3) 2_566
C3 C5 1.516(3) .
C6 C7 1.507(4) 2_556
C7 C6 1.507(4) 2_556
