#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:11:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179279 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319997.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_4319997
loop_
_publ_author_name
'Eringathodi Suresh'
'Kamla Boopalan'
'Raksh Vir Jasra'
'Mohan Madhav Bhadbhade'
_publ_section_title
;
 Synthesis and Single Crystal Investigation of Two-Dimensional Rectangular
 Network [M(4,4'-bpy) (Phth)(H2O)]n.2H2O with Small Neutral Cavities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4078
_journal_page_last               4080
_journal_paper_doi               10.1021/ic000434v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C18 H20 Co N2 O8'
_chemical_formula_weight         451.29
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 92.51(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.596(3)
_cell_length_b                   11.309(3)
_cell_length_c                   10.770(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8
_cell_volume                     924.3(5)
_computing_cell_refinement       CAD4-PC
_computing_data_collection       CAD4-PC
_computing_data_reduction        NRCVAX
_computing_molecular_graphics    'PLUTON, ORTEP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-two theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1629
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.61
_diffrn_standards_interval_time  1h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   'empirical absorption correction(NRCVAX)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.702
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1160P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                1300
_reflns_number_total             1629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000434v_1.cif
_cod_data_source_block           001jas_[co(44bpy)(phth)].2H2O_complex-1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319997
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.7500 0.72021(6) 0.7500 0.0187(3) Uani 1 d S . .
N2 N 0.7500 0.5313(4) 0.7500 0.0236(10) Uani 1 d S . .
C7 C 1.1296(5) 0.7269(3) 0.6394(4) 0.0220(8) Uani 1 d . . .
N1 N 0.7500 0.9069(4) 0.7500 0.0204(10) Uani 1 d S . .
C1 C 0.8151(5) 0.9700(4) 0.8471(4) 0.0258(9) Uani 1 d . . .
O1 O 0.9655(3) 0.7088(2) 0.6296(3) 0.0293(7) Uani 1 d . . .
C5 C 0.6022(5) 0.4697(3) 0.7277(4) 0.0274(10) Uani 1 d . . .
O1W O 0.5835(4) 0.7181(2) 0.5873(3) 0.0242(6) Uani 1 d . . .
O2 O 1.2420(4) 0.6590(3) 0.6000(3) 0.0406(9) Uani 1 d . . .
C3 C 0.7500 1.1548(5) 0.7500 0.0232(12) Uani 1 d S . .
C8 C 1.1911(5) 0.8407(3) 0.6988(3) 0.0180(8) Uani 1 d . . .
C2 C 0.8179(5) 1.0917(4) 0.8506(4) 0.0262(9) Uani 1 d . . .
C9 C 1.1384(5) 0.9474(4) 0.6468(4) 0.0298(10) Uani 1 d . . .
C4 C 0.7500 1.2848(5) 0.7500 0.0232(12) Uani 1 d S . .
C6 C 0.5968(5) 0.3486(4) 0.7241(4) 0.0269(9) Uani 1 d . . .
C10 C 1.1947(6) 1.0527(4) 0.6976(5) 0.0378(11) Uani 1 d . . .
O2W O 0.7848(5) 0.5874(4) 0.4367(4) 0.0434(9) Uani 1 d . . .
H1 H 0.847(7) 0.929(5) 0.917(5) 0.043(14) Uiso 1 d . . .
H10 H 1.161(7) 1.117(5) 0.663(5) 0.053(17) Uiso 1 d . . .
H1O1 H 0.482(8) 0.715(5) 0.589(6) 0.056(19) Uiso 1 d . . .
H2 H 0.849(6) 1.137(4) 0.918(5) 0.041(13) Uiso 1 d . . .
H6 H 0.494(5) 0.319(4) 0.706(4) 0.024(11) Uiso 1 d . . .
H2O1 H 0.621(6) 0.677(4) 0.534(4) 0.028(13) Uiso 1 d . . .
H5 H 0.501(6) 0.509(4) 0.713(4) 0.028(11) Uiso 1 d . . .
H9 H 1.062(7) 0.943(4) 0.578(5) 0.048(15) Uiso 1 d . . .
H2O2 H 0.798(11) 0.514(7) 0.418(7) 0.10(3) Uiso 1 d . . .
H1O2 H 0.853(8) 0.602(5) 0.478(6) 0.05(2) Uiso 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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'
N N 0.0061 0.0033 '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'
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
_geom_angle_publ_flag
N1 Co1 O1W 90.64(8) . 2_656 ?
N1 Co1 O1W 90.64(8) . . ?
O1W Co1 O1W 178.73(16) 2_656 . ?
N1 Co1 O1 93.45(8) . 2_656 ?
O1W Co1 O1 86.73(12) 2_656 2_656 ?
O1W Co1 O1 93.19(12) . 2_656 ?
N1 Co1 O1 93.45(8) . . ?
O1W Co1 O1 93.19(12) 2_656 . ?
O1W Co1 O1 86.73(12) . . ?
O1 Co1 O1 173.10(15) 2_656 . ?
N1 Co1 N2 180.000(1) . . ?
O1W Co1 N2 89.36(8) 2_656 . ?
O1W Co1 N2 89.36(8) . . ?
O1 Co1 N2 86.55(8) 2_656 . ?
O1 Co1 N2 86.55(8) . . ?
C5 N2 C5 117.0(5) . 2_656 ?
C5 N2 Co1 121.5(2) . . ?
C5 N2 Co1 121.5(2) 2_656 . ?
O2 C7 O1 124.4(4) . . ?
O2 C7 C8 118.1(3) . . ?
O1 C7 C8 117.5(3) . . ?
C1 N1 C1 115.8(5) . 2_656 ?
C1 N1 Co1 122.1(2) . . ?
C1 N1 Co1 122.1(2) 2_656 . ?
N1 C1 C2 123.9(4) . . ?
C7 O1 Co1 136.0(3) . . ?
N2 C5 C6 123.4(4) . . ?
C2 C3 C2 117.6(5) 2_656 . ?
C2 C3 C4 121.2(3) 2_656 . ?
C2 C3 C4 121.2(3) . . ?
C9 C8 C8 119.1(3) . 2_756 ?
C9 C8 C7 119.7(4) . . ?
C8 C8 C7 121.0(2) 2_756 . ?
C1 C2 C3 119.4(4) . . ?
C10 C9 C8 121.1(4) . . ?
C6 C4 C6 117.3(5) 1_565 2_666 ?
C6 C4 C3 121.3(2) 1_565 . ?
C6 C4 C3 121.3(2) 2_666 . ?
C5 C6 C4 119.3(4) . 1_545 ?
C9 C10 C10 119.7(3) . 2_756 ?
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
Co1 N1 2.111(4) . ?
Co1 O1W 2.116(3) 2_656 ?
Co1 O1W 2.116(3) . ?
Co1 O1 2.136(3) 2_656 ?
Co1 O1 2.136(3) . ?
Co1 N2 2.137(5) . ?
N2 C5 1.334(5) . ?
N2 C5 1.334(5) 2_656 ?
C7 O2 1.237(5) . ?
C7 O1 1.263(5) . ?
C7 C8 1.503(5) . ?
N1 C1 1.343(5) . ?
N1 C1 1.343(5) 2_656 ?
C1 C2 1.376(6) . ?
C5 C6 1.371(5) . ?
C3 C2 1.379(5) 2_656 ?
C3 C2 1.379(5) . ?
C3 C4 1.471(7) . ?
C8 C9 1.382(6) . ?
C8 C8 1.390(7) 2_756 ?
C9 C10 1.371(7) . ?
C4 C6 1.387(5) 1_565 ?
C4 C6 1.387(5) 2_666 ?
C6 C4 1.387(5) 1_545 ?
C10 C10 1.377(10) 2_756 ?
