#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312698.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_4312698
loop_
_publ_author_name
'Yanjuan Qi'
'Yonghui Wang'
'Changwen Hu'
'Minhua Cao'
'Li Mao'
'Enbo Wang'
_publ_section_title
;
 A New Type of Single-Helix Coordination Polymer with Mixed Ligands
 [M2(phen)2(e,a-cis-1,4-chdc)2(H2O)2]n (M = Co and Ni; phen =
 1,10-phenanthroline; chdc = cyclohexanedicarboxylate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8519
_journal_page_last               8523
_journal_paper_doi               10.1021/ic034796p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C40 H36 N4 Ni2 O10'
_chemical_formula_weight         850.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.31(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8921(6)
_cell_length_b                   9.0151(4)
_cell_length_c                   20.1628(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1769.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6747
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.133
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                2574
_reflns_number_total             3810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034796psi20031002_084516.cif
_cod_data_source_block           dss343
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1769.0(2)
_cod_database_code               4312698
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.69481(4) -0.55454(4) 0.60593(2) 0.02348(11) Uani 1 1 d . . .
O1 O 0.6233(2) -0.5475(2) 0.69443(11) 0.0368(5) Uani 1 1 d . . .
O2 O 0.4235(2) -0.6646(3) 0.66397(13) 0.0452(6) Uani 1 1 d . . .
O3 O 0.23614(19) -0.8322(2) 0.87295(11) 0.0281(5) Uani 1 1 d . . .
O4 O 0.43221(18) -0.8780(2) 0.93854(11) 0.0271(5) Uani 1 1 d . . .
OW O 0.55831(19) -0.7191(2) 0.56721(11) 0.0299(5) Uani 1 1 d . . .
N1 N 0.7915(2) -0.5864(2) 0.52324(13) 0.0245(6) Uani 1 1 d . . .
N2 N 0.8617(2) -0.6801(3) 0.65027(13) 0.0267(6) Uani 1 1 d . . .
C1 C 0.7546(3) -0.5385(3) 0.46069(17) 0.0316(7) Uani 1 1 d . . .
H1 H 0.6789 -0.4759 0.4507 0.038 Uiso 1 1 calc R . .
C2 C 0.8246(3) -0.5779(4) 0.40899(18) 0.0414(9) Uani 1 1 d . . .
H2 H 0.7960 -0.5415 0.3656 0.050 Uiso 1 1 calc R . .
C3 C 0.9350(3) -0.6700(4) 0.42272(19) 0.0453(9) Uani 1 1 d . . .
H3 H 0.9821 -0.6973 0.3886 0.054 Uiso 1 1 calc R . .
C4 C 0.9776(3) -0.7239(3) 0.48862(18) 0.0343(8) Uani 1 1 d . . .
C5 C 0.9017(3) -0.6790(3) 0.53751(16) 0.0255(7) Uani 1 1 d . . .
C6 C 0.9410(3) -0.7267(3) 0.60533(16) 0.0261(7) Uani 1 1 d . . .
C7 C 1.0581(3) -0.8156(3) 0.62445(18) 0.0321(8) Uani 1 1 d . . .
C8 C 1.0939(3) -0.8546(4) 0.6920(2) 0.0424(9) Uani 1 1 d . . .
H8 H 1.1719 -0.9117 0.7067 0.051 Uiso 1 1 calc R . .
C9 C 1.0143(3) -0.8087(4) 0.73620(18) 0.0428(9) Uani 1 1 d . . .
H9 H 1.0367 -0.8347 0.7815 0.051 Uiso 1 1 calc R . .
C10 C 0.8977(3) -0.7218(3) 0.71311(18) 0.0358(8) Uani 1 1 d . . .
H10 H 0.8434 -0.6923 0.7440 0.043 Uiso 1 1 calc R . .
C11 C 1.0936(3) -0.8184(4) 0.5087(2) 0.0484(10) Uani 1 1 d . . .
H11 H 1.1429 -0.8521 0.4764 0.058 Uiso 1 1 calc R . .
C12 C 1.1327(3) -0.8597(4) 0.5733(2) 0.0472(10) Uani 1 1 d . . .
H12 H 1.2105 -0.9185 0.5850 0.057 Uiso 1 1 calc R . .
C13 C 0.5094(3) -0.5919(3) 0.70568(17) 0.0302(7) Uani 1 1 d . . .
C14 C 0.4770(3) -0.5524(3) 0.77480(16) 0.0327(7) Uani 1 1 d . . .
C15 C 0.3269(3) -0.5722(4) 0.77960(17) 0.0355(8) Uani 1 1 d . . .
H15A H 0.3002 -0.6740 0.7685 0.043 Uiso 1 1 calc R . .
H15B H 0.2715 -0.5084 0.7467 0.043 Uiso 1 1 calc R . .
C16 C 0.2975(3) -0.5363(3) 0.84876(16) 0.0306(7) Uani 1 1 d . . .
H16A H 0.3116 -0.4310 0.8571 0.037 Uiso 1 1 calc R . .
H16B H 0.2018 -0.5579 0.8496 0.037 Uiso 1 1 calc R . .
C17 C 0.3873(3) -0.6226(3) 0.90537(16) 0.0241(7) Uani 1 1 d . . .
C18 C 0.5396(3) -0.6032(3) 0.89913(16) 0.0266(7) Uani 1 1 d . . .
H18A H 0.5664 -0.5009 0.9088 0.032 Uiso 1 1 calc R . .
H18B H 0.5960 -0.6653 0.9324 0.032 Uiso 1 1 calc R . .
C19 C 0.5665(3) -0.6435(3) 0.82964(16) 0.0291(7) Uani 1 1 d . . .
H19A H 0.5478 -0.7481 0.8214 0.035 Uiso 1 1 calc R . .
H19B H 0.6626 -0.6261 0.8278 0.035 Uiso 1 1 calc R . .
C20 C 0.3495(3) -0.7860(3) 0.90490(15) 0.0230(6) 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
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
_geom_angle_publ_flag
O1 Ni OW 92.72(9) . . ?
O1 Ni N2 90.79(9) . . ?
OW Ni N2 100.83(9) . . ?
O1 Ni N1 170.65(9) . . ?
OW Ni N1 87.77(9) . . ?
N2 Ni N1 79.96(10) . . ?
O1 Ni O4 94.28(8) . 2_656 ?
OW Ni O4 94.66(7) . 2_656 ?
N2 Ni O4 163.45(8) . 2_656 ?
N1 Ni O4 94.98(9) . 2_656 ?
O1 Ni O3 86.85(9) . 2_656 ?
OW Ni O3 156.15(7) . 2_656 ?
N2 Ni O3 103.02(8) . 2_656 ?
N1 Ni O3 96.47(8) . 2_656 ?
O4 Ni O3 61.64(7) 2_656 2_656 ?
O1 Ni C20 87.88(9) . 2_656 ?
OW Ni C20 125.39(8) . 2_656 ?
N2 Ni C20 133.77(9) . 2_656 ?
N1 Ni C20 99.45(9) . 2_656 ?
O4 Ni C20 31.10(8) 2_656 2_656 ?
O3 Ni C20 30.76(8) 2_656 2_656 ?
C13 O1 Ni 127.8(2) . . ?
C20 O3 Ni 89.16(16) . 2_646 ?
C20 O4 Ni 89.32(16) . 2_646 ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Ni 129.09(19) . . ?
C5 N1 Ni 112.3(2) . . ?
C10 N2 C6 117.7(3) . . ?
C10 N2 Ni 129.3(2) . . ?
C6 N2 Ni 112.97(19) . . ?
N1 C1 C2 122.7(3) . . ?
C3 C2 C1 119.4(3) . . ?
C2 C3 C4 119.8(3) . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C11 118.5(3) . . ?
C3 C4 C11 124.3(3) . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 117.4(3) . . ?
C4 C5 C6 120.1(3) . . ?
N2 C6 C7 122.5(3) . . ?
N2 C6 C5 117.1(2) . . ?
C7 C6 C5 120.5(3) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 124.3(3) . . ?
C6 C7 C12 117.9(3) . . ?
C9 C8 C7 119.4(3) . . ?
C8 C9 C10 119.5(3) . . ?
N2 C10 C9 123.2(3) . . ?
C12 C11 C4 121.1(3) . . ?
C11 C12 C7 121.8(3) . . ?
O1 C13 O2 124.2(3) . . ?
O1 C13 C14 115.7(3) . . ?
O2 C13 C14 120.1(3) . . ?
C13 C14 C15 113.5(3) . . ?
C13 C14 C19 110.3(2) . . ?
C15 C14 C19 109.8(3) . . ?
C14 C15 C16 112.7(3) . . ?
C17 C16 C15 113.5(2) . . ?
C20 C17 C16 112.3(2) . . ?
C20 C17 C18 110.6(2) . . ?
C16 C17 C18 109.1(2) . . ?
C19 C18 C17 112.5(2) . . ?
C18 C19 C14 111.4(2) . . ?
O3 C20 O4 119.0(2) . . ?
O3 C20 C17 121.3(2) . . ?
O4 C20 C17 119.6(2) . . ?
O3 C20 Ni 60.08(14) . 2_646 ?
O4 C20 Ni 59.58(14) . 2_646 ?
C17 C20 Ni 173.3(2) . 2_646 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni O1 2.035(2) . ?
Ni OW 2.0629(19) . ?
Ni N2 2.068(2) . ?
Ni N1 2.085(3) . ?
Ni O4 2.1244(19) 2_656 ?
Ni O3 2.1353(19) 2_656 ?
Ni C20 2.463(3) 2_656 ?
O1 C13 1.254(3) . ?
O2 C13 1.266(4) . ?
O3 C20 1.260(3) . ?
O3 Ni 2.1353(18) 2_646 ?
O4 C20 1.273(3) . ?
O4 Ni 2.1244(19) 2_646 ?
N1 C1 1.321(4) . ?
N1 C5 1.363(3) . ?
N2 C10 1.308(4) . ?
N2 C6 1.367(4) . ?
C1 C2 1.397(4) . ?
C2 C3 1.360(5) . ?
C3 C4 1.407(5) . ?
C4 C5 1.401(4) . ?
C4 C11 1.428(4) . ?
C5 C6 1.420(4) . ?
C6 C7 1.404(4) . ?
C7 C8 1.390(5) . ?
C7 C12 1.428(5) . ?
C8 C9 1.356(5) . ?
C9 C10 1.403(4) . ?
C11 C12 1.344(5) . ?
C13 C14 1.527(4) . ?
C14 C15 1.515(4) . ?
C14 C19 1.527(4) . ?
C15 C16 1.510(4) . ?
C16 C17 1.528(4) . ?
C17 C20 1.519(4) . ?
C17 C18 1.544(4) . ?
C18 C19 1.516(4) . ?
C20 Ni 2.463(3) 2_646 ?
