#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:30:10 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243950 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702685.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_7702685
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         '[Zn(H2O)4(C6H2(COO)4)]2-(C4H12N)2+(H2O)2'
_chemical_formula_sum            'C14 H30 N2 O16 Zn'
_chemical_formula_weight         547.77
_chemical_name_common            'Zn_Pyromelttate coordination 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                104.870(10)
_cell_angle_beta                 98.16(3)
_cell_angle_gamma                109.45(3)
_cell_formula_units_Z            1
_cell_length_a                   6.847(5)
_cell_length_b                   9.1220(10)
_cell_length_c                   9.769(2)
_cell_measurement_reflns_used    3
_cell_measurement_temperature    293(2)
_cell_volume                     538.5(4)
_computing_cell_refinement       'nonius mach3 software'
_computing_data_collection       'nonius mach3 software'
_computing_data_reduction        'nonius maxus'
_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  0.0080
_diffrn_reflns_av_sigmaI/netI    0.0126
_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       -3
_diffrn_reflns_number            2067
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.6399
_exptl_absorpt_correction_T_min  0.5268
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0343
_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)+(0.0540P)²+0.5486P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                1866
_reflns_number_total             1889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105687p.txt
_cod_data_source_block           rm004
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702685
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
Zn1 Zn 0.0000 0.0000 0.0000 0.02030(16) Uani 1 d S
O1 O 0.2557(3) 0.1729(2) -0.0429(2) 0.0267(4) Uani 1 d .
O2 O 0.2045(3) -0.0966(2) 0.08534(19) 0.0220(4) Uani 1 d .
O3 O 0.0296(3) 0.16174(19) 0.21539(17) 0.0199(4) Uani 1 d .
O4 O 0.2780(5) 0.3950(3) 0.2220(4) 0.0829(12) Uani 1 d .
O5 O -0.3446(3) 0.2553(2) 0.13180(18) 0.0239(4) Uani 1 d .
O6 O -0.4621(3) 0.1255(2) 0.2871(2) 0.0334(5) Uani 1 d .
O7 O 0.4078(4) -0.2709(3) 0.2653(3) 0.0500(6) Uani 1 d .
O8 O -0.1365(17) -0.4505(5) 0.0807(6) 0.144(3) Uani 1 d .
N1 N -0.1730(4) -0.0506(3) 0.3730(2) 0.0272(5) Uani 1 d .
C1 C 0.2132(4) 0.5405(3) 0.5012(3) 0.0199(5) Uani 1 d .
C2 C 0.0579(4) 0.4117(3) 0.3839(2) 0.0183(5) Uani 1 d .
C3 C -0.1575(4) 0.3720(3) 0.3829(2) 0.0174(5) Uani 1 d .
C4 C 0.1285(4) 0.3166(3) 0.2641(3) 0.0252(5) Uani 1 d .
C5 C -0.3356(4) 0.2388(3) 0.2568(3) 0.0196(5) Uani 1 d .
C6 C -0.0320(5) -0.1442(4) 0.3809(3) 0.0327(6) Uani 1 d .
C7 C -0.1867(5) 0.0329(4) 0.5216(3) 0.0321(6) Uani 1 d .
H1 H 0.391(8) 0.185(6) 0.009(6) 0.080 Uiso 1 d .
H2 H 0.249(8) 0.260(7) -0.022(6) 0.080 Uiso 1 d .
H3 H 0.247(8) -0.147(6) 0.012(6) 0.080 Uiso 1 d .
H4 H 0.304(8) -0.023(6) 0.148(6) 0.080 Uiso 1 d .
H5 H 0.363(8) 0.568(6) 0.510(5) 0.080 Uiso 1 d .
H6 H -0.128(8) 0.020(6) 0.326(6) 0.080 Uiso 1 d .
H7 H -0.319(8) -0.137(6) 0.315(6) 0.080 Uiso 1 d .
H8 H -0.016(8) -0.199(6) 0.274(6) 0.080 Uiso 1 d .
H9 H -0.099(8) -0.232(6) 0.416(6) 0.080 Uiso 1 d .
H10 H -0.260(8) 0.097(6) 0.515(5) 0.080 Uiso 1 d .
H11 H -0.254(8) -0.053(6) 0.563(6) 0.080 Uiso 1 d .
H12 H 0.387(8) -0.374(7) 0.242(6) 0.080 Uiso 1 d .
H13 H 0.306(8) -0.270(6) 0.194(6) 0.080 Uiso 1 d .
H14 H -0.107(12) -0.507(8) 0.080(8) 0.080 Uiso 1 d .
H15 H -0.254(9) -0.496(8) 0.068(7) 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'
Zn Zn 0.2839 1.4301 '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 Zn1 O2 180.00(11) 2 .
O2 Zn1 O1 89.13(9) 2 .
O2 Zn1 O1 90.87(9) . .
O2 Zn1 O1 90.87(9) 2 2
O2 Zn1 O1 89.13(9) . 2
O1 Zn1 O1 180.00(11) . 2
O2 Zn1 O3 87.82(7) 2 .
O2 Zn1 O3 92.18(7) . .
O1 Zn1 O3 94.63(7) . .
O1 Zn1 O3 85.37(7) 2 .
O2 Zn1 O3 92.18(7) 2 2
O2 Zn1 O3 87.82(7) . 2
O1 Zn1 O3 85.37(7) . 2
O1 Zn1 O3 94.63(7) 2 2
O3 Zn1 O3 180.00(10) . 2
C4 O3 Zn1 126.40(16) . .
C7 N1 C6 111.0(2) . .
C3 C1 C2 121.4(2) 2_566 .
C3 C2 C1 119.1(2) . .
C3 C2 C4 121.9(2) . .
C1 C2 C4 119.0(2) . .
C1 C3 C2 119.5(2) 2_566 .
C1 C3 C5 118.2(2) 2_566 .
C2 C3 C5 122.3(2) . .
O4 C4 O3 125.1(2) . .
O4 C4 C2 117.6(2) . .
O3 C4 C2 117.3(2) . .
O6 C5 O5 126.1(2) . .
O6 C5 C3 116.6(2) . .
O5 C5 C3 117.3(2) . .
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
Zn1 O2 2.0733(19) 2
Zn1 O2 2.0733(19) .
Zn1 O1 2.106(2) .
Zn1 O1 2.106(2) 2
Zn1 O3 2.1751(16) .
Zn1 O3 2.1751(16) 2
O3 C4 1.268(3) .
O4 C4 1.230(4) .
O5 C5 1.264(3) .
O6 C5 1.241(3) .
N1 C7 1.489(4) .
N1 C6 1.493(4) .
C1 C3 1.387(3) 2_566
C1 C2 1.398(3) .
C2 C3 1.395(4) .
C2 C4 1.508(3) .
C3 C1 1.387(3) 2_566
C3 C5 1.516(3) .
C6 C7 1.506(4) 2_556
C7 C6 1.506(4) 2_556
