#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/46/4504614.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_4504614
loop_
_publ_author_name
'Chen, Jinxi'
'Ohba, Masaaki'
'Zhao, Dongyuan'
'Kaneko, Wakako'
'Kitagawa, Susumu'
_publ_section_title
;
 Polynuclear Core-Based Nickel 1,4-Cyclohexanedicarboxylate Coordination
 Polymers as Temperature-Dependent Hydrothermal Reaction Products
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              664
_journal_paper_doi               10.1021/cg050363g
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C4 H5 Ni0.75 O4.5'
_chemical_formula_weight         169.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.086(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0967(10)
_cell_length_b                   9.9992(5)
_cell_length_c                   6.3722(4)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.22
_cell_volume                     1270.72(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4957
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            gree
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0408
_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)+(0.0589P)²+7.1849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                1472
_reflns_number_total             1506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050363gsi20050725_102742.cif
_cod_data_source_block           Ni3(OH)2(CDC)2(H2O)4.4(H2O)
_cod_original_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'C4 H5 Ni0.75 O4.50'
_cod_database_code               4504614
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -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
Ni2 Ni 0.0000 -0.15118(5) 0.5000 0.00916(19) Uani 1 2 d S
Ni1 Ni 0.0000 0.0000 0.0000 0.0078(2) Uani 1 4 d S
O1 O 0.09511(10) -0.1653(2) 0.6549(3) 0.0170(5) Uani 1 1 d .
O2 O 0.07254(10) -0.1476(2) 0.9888(3) 0.0150(4) Uani 1 1 d .
O3 O 0.02899(13) 0.0000 0.3170(4) 0.0091(5) Uani 1 2 d S
O4 O 0.03376(11) -0.3013(2) 0.3002(3) 0.0177(4) Uani 1 1 d .
O5 O 0.1240(2) -0.5000 0.4687(8) 0.0478(11) Uani 1 2 d S
O6 O 0.0593(2) -0.5000 0.8418(8) 0.0482(11) Uani 1 2 d S
C1 C 0.18213(19) -0.2137(8) 0.9297(6) 0.0645(19) Uani 1 1 d .
H1 H 0.1707 -0.3090 0.9234 0.077 Uiso 1 1 calc R
C2 C 0.20326(19) -0.2189(8) 1.1481(6) 0.0625(19) Uani 1 1 d .
H2A H 0.1710 -0.2725 1.2122 0.075 Uiso 1 1 calc R
H2B H 0.2007 -0.1289 1.2033 0.075 Uiso 1 1 calc R
C3 C 0.22839(18) -0.2276(6) 0.7762(5) 0.0497(14) Uani 1 1 d .
H3A H 0.2338 -0.1405 0.7136 0.060 Uiso 1 1 calc R
H3B H 0.2081 -0.2859 0.6646 0.060 Uiso 1 1 calc R
C4 C 0.11138(13) -0.1724(3) 0.8503(4) 0.0135(5) 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
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
O3 Ni2 O3 84.22(10) 5_556 .
O3 Ni2 O1 90.64(9) 5_556 6_556
O3 Ni2 O1 95.23(9) . 6_556
O3 Ni2 O1 95.23(9) 5_556 .
O3 Ni2 O1 90.64(9) . .
O1 Ni2 O1 172.09(13) 6_556 .
O3 Ni2 O4 176.72(8) 5_556 .
O3 Ni2 O4 92.64(8) . .
O1 Ni2 O4 90.61(8) 6_556 .
O1 Ni2 O4 83.82(8) . .
O3 Ni2 O4 92.64(8) 5_556 6_556
O3 Ni2 O4 176.72(8) . 6_556
O1 Ni2 O4 83.82(8) 6_556 6_556
O1 Ni2 O4 90.61(8) . 6_556
O4 Ni2 O4 90.50(12) . 6_556
O3 Ni1 O3 180.0 5 .
O3 Ni1 O2 85.30(8) 5 6_556
O3 Ni1 O2 94.70(8) . 6_556
O3 Ni1 O2 94.70(8) 5 2_554
O3 Ni1 O2 85.30(8) . 2_554
O2 Ni1 O2 180.00(11) 6_556 2_554
O3 Ni1 O2 94.70(8) 5 1_554
O3 Ni1 O2 85.30(8) . 1_554
O2 Ni1 O2 89.71(12) 6_556 1_554
O2 Ni1 O2 90.29(12) 2_554 1_554
O3 Ni1 O2 85.30(8) 5 5_556
O3 Ni1 O2 94.70(8) . 5_556
O2 Ni1 O2 90.29(12) 6_556 5_556
O2 Ni1 O2 89.71(12) 2_554 5_556
O2 Ni1 O2 180.00(11) 1_554 5_556
C4 O1 Ni2 126.78(18) . .
C4 O2 Ni1 130.85(19) . 1_556
Ni1 O3 Ni2 120.12(8) . 5_556
Ni1 O3 Ni2 120.12(8) . .
Ni2 O3 Ni2 95.78(10) 5_556 .
C2 C1 C3 121.9(3) . .
C2 C1 C4 120.0(3) . .
C3 C1 C4 117.4(3) . .
C1 C2 C3 119.0(3) . 7_547
C1 C3 C2 117.4(3) . 7_547
O1 C4 O2 124.9(3) . .
O1 C4 C1 118.1(3) . .
O2 C4 C1 117.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni2 O3 2.0377(17) 5_556
Ni2 O3 2.0377(17) .
Ni2 O1 2.045(2) 6_556
Ni2 O1 2.045(2) .
Ni2 O4 2.133(2) .
Ni2 O4 2.133(2) 6_556
Ni1 O3 2.032(2) 5
Ni1 O3 2.032(2) .
Ni1 O2 2.0819(19) 6_556
Ni1 O2 2.0819(19) 2_554
Ni1 O2 2.0819(19) 1_554
Ni1 O2 2.0819(19) 5_556
O1 C4 1.250(3) .
O2 C4 1.272(3) .
O2 Ni1 2.0819(19) 1_556
O3 Ni2 2.0377(17) 5_556
C1 C2 1.405(5) .
C1 C3 1.437(4) .
C1 C4 1.507(4) .
C2 C3 1.497(5) 7_547
C3 C2 1.497(5) 7_547
