#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310791.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_4310791
loop_
_publ_author_name
'Xi-Xue Hu'
'Ji-Qing Xu'
'Peng Cheng'
'Xiao-Yan Chen'
'Xiao-Bing Cui'
'Jiang-Feng Song'
'Guang-Di Yang'
'Tie-Gang Wang'
_publ_section_title
;
 A New Route for Preparing Coordination Polymers from Hydrothermal
 Reactions Involving in Situ Ligand Synthesis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2261
_journal_page_last               2266
_journal_paper_doi               10.1021/ic0351646
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C19 H12 Co N4 O4'
_chemical_formula_sum            'C19 H12 Co N4 O4'
_chemical_formula_weight         419.26
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 117.677(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9464(13)
_cell_length_b                   23.685(5)
_cell_length_c                   7.9491(16)
_cell_measurement_temperature    293(2)
_cell_volume                     1658.4(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_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  'Siemens P4 diffractometer'
_diffrn_measurement_method       w-scan
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2059
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.072
_exptl_crystal_colour            deep_red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         1921
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                1827
_reflns_number_total             1921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351646si20031008_025554.cif
_cod_data_source_block           h
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1658.4(5)
_cod_database_code               4310791
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -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
Co1 Co 0.45567(6) 0.389008(14) 0.28928(6) 0.02497(12) Uani 1 1 d . . .
C1 C 0.3248(5) 0.37422(17) -0.1494(6) 0.0398(9) Uani 1 1 d . . .
C2 C 0.2711(6) 0.3454(2) -0.3212(6) 0.0496(11) Uani 1 1 d . . .
C3 C 0.2671(6) 0.2883(2) -0.3170(7) 0.0542(12) Uani 1 1 d . . .
C4 C 0.3163(5) 0.26026(17) -0.1466(6) 0.0433(10) Uani 1 1 d . . .
C5 C 0.3688(5) 0.29155(18) 0.0195(7) 0.0332(9) Uani 1 1 d . . .
C6 C 0.4274(4) 0.26625(15) 0.2104(6) 0.0314(8) Uani 1 1 d . . .
C7 C 0.4315(6) 0.20813(16) 0.2405(7) 0.0469(12) Uani 1 1 d . . .
C8 C 0.4925(7) 0.1882(2) 0.4229(9) 0.0557(13) Uani 1 1 d . . .
C9 C 0.5435(6) 0.2248(2) 0.5718(7) 0.0535(12) Uani 1 1 d . . .
C10 C 0.5368(6) 0.2828(2) 0.5335(7) 0.0386(11) Uani 1 1 d . . .
C11 C 0.7058(4) 0.41860(15) 0.2129(5) 0.0318(8) Uani 1 1 d . . .
C12 C 0.8103(4) 0.45639(14) 0.1837(5) 0.0246(6) Uani 1 1 d . . .
C13 C 0.9503(4) 0.43611(14) 0.2067(5) 0.0281(7) Uani 1 1 d . . .
C14 C 1.0528(4) 0.47228(16) 0.1921(5) 0.0283(7) Uani 1 1 d . . .
C15 C 1.0160(4) 0.52985(16) 0.1544(6) 0.0322(8) Uani 1 1 d . . .
C16 C 0.8795(4) 0.55034(14) 0.1334(5) 0.0291(7) Uani 1 1 d . . .
C17 C 0.7757(4) 0.51379(14) 0.1471(5) 0.0230(6) Uani 1 1 d . . .
C18 C 0.2050(4) 0.4533(2) 0.2145(5) 0.0379(9) Uani 1 1 d . . .
C19 C 0.6275(4) 0.46569(14) 0.6194(4) 0.0242(7) Uani 1 1 d . . .
O1 O 0.2898(4) 0.48829(19) 0.1963(6) 0.0665(11) Uani 1 1 d . . .
O2 O 0.2391(4) 0.40124(16) 0.2532(5) 0.0512(8) Uani 1 1 d . . .
O3 O 0.5805(3) 0.41574(10) 0.5710(4) 0.0312(5) Uani 1 1 d . . .
O4 O 0.7364(4) 0.36775(12) 0.2601(5) 0.0500(8) Uani 1 1 d . . .
N1 N 0.4786(3) 0.30305(13) 0.3577(4) 0.0296(6) Uani 1 1 d . . .
N2 N 0.3691(3) 0.34840(12) 0.0177(5) 0.0294(6) Uani 1 1 d . . .
N3 N 0.5447(3) 0.49665(13) 0.1522(4) 0.0278(6) Uani 1 1 d . . .
N4 N 0.5780(3) 0.44022(13) 0.2017(4) 0.0306(7) Uani 1 1 d . . .
H12 H 0.587(6) 0.2089(19) 0.709(6) 0.033(13) Uiso 1 1 d . . .
H11 H 0.338(8) 0.216(3) -0.108(10) 0.08(2) Uiso 1 1 d . . .
H10 H 0.969(5) 0.3932(16) 0.240(5) 0.027(11) Uiso 1 1 d . . .
H9 H 1.073(5) 0.5531(17) 0.138(6) 0.026(10) Uiso 1 1 d . . .
H8 H 0.551(6) 0.314(2) 0.612(7) 0.041(13) Uiso 1 1 d . . .
H7 H 0.860(6) 0.590(2) 0.119(7) 0.043(12) Uiso 1 1 d . . .
H6 H 0.340(6) 0.417(2) -0.134(8) 0.057(15) Uiso 1 1 d . . .
H5 H 0.250(7) 0.361(3) -0.424(9) 0.062(17) Uiso 1 1 d . . .
H4 H 0.467(6) 0.5047(19) 0.151(6) 0.033(11) Uiso 1 1 d . . .
H3 H 0.235(9) 0.272(3) -0.438(11) 0.10(3) Uiso 1 1 d . . .
H2 H 0.514(9) 0.145(3) 0.477(11) 0.10(2) Uiso 1 1 d . . .
H1 H 0.391(9) 0.185(3) 0.101(10) 0.08(2) Uiso 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'
Co Co 0.3494 0.9721 '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
O2 Co1 N4 128.02(14) . . ?
O2 Co1 O3 99.75(12) . . ?
N4 Co1 O3 91.93(11) . . ?
O2 Co1 N1 98.87(14) . . ?
N4 Co1 N1 130.69(12) . . ?
O3 Co1 N1 94.45(11) . . ?
O2 Co1 N2 91.01(13) . . ?
N4 Co1 N2 87.01(13) . . ?
O3 Co1 N2 167.06(11) . . ?
N1 Co1 N2 76.67(12) . . ?
N2 C1 C2 123.3(4) . . ?
C3 C2 C1 117.9(4) . . ?
C2 C3 C4 120.2(4) . . ?
C3 C4 C5 118.9(4) . . ?
N2 C5 C4 121.7(4) . . ?
N2 C5 C6 114.5(4) . . ?
C4 C5 C6 123.8(4) . . ?
N1 C6 C7 121.1(4) . . ?
N1 C6 C5 116.0(3) . . ?
C7 C6 C5 122.9(4) . . ?
C8 C7 C6 119.0(4) . . ?
C9 C8 C7 120.3(4) . . ?
C8 C9 C10 118.3(4) . . ?
N1 C10 C9 122.3(5) . . ?
O4 C11 N4 118.6(3) . . ?
O4 C11 C12 122.7(3) . . ?
N4 C11 C12 118.5(3) . . ?
C17 C12 C13 119.6(3) . . ?
C17 C12 C11 120.0(3) . . ?
C13 C12 C11 120.2(3) . . ?
C14 C13 C12 120.3(3) . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 C18 123.1(3) . 1_655 ?
C15 C14 C18 117.4(4) . 1_655 ?
C16 C15 C14 120.7(3) . . ?
C15 C16 C17 119.8(3) . . ?
C16 C17 C12 120.1(3) . . ?
C16 C17 C19 120.9(3) . 2_564 ?
C12 C17 C19 119.1(3) . 2_564 ?
O1 C18 O2 123.7(4) . . ?
O1 C18 C14 119.2(4) . 1_455 ?
O2 C18 C14 117.1(4) . 1_455 ?
O3 C19 N3 121.1(3) . 2_565 ?
O3 C19 C17 123.9(3) . 2_565 ?
N3 C19 C17 115.0(3) 2_565 2_565 ?
C18 O2 Co1 108.2(3) . . ?
C19 O3 Co1 124.1(2) . . ?
C10 N1 C6 118.8(4) . . ?
C10 N1 Co1 124.4(3) . . ?
C6 N1 Co1 116.7(2) . . ?
C1 N2 C5 117.8(4) . . ?
C1 N2 Co1 126.0(3) . . ?
C5 N2 Co1 116.1(3) . . ?
C19 N3 N4 128.1(3) 2_564 . ?
C11 N4 N3 118.9(3) . . ?
C11 N4 Co1 116.5(2) . . ?
N3 N4 Co1 124.2(2) . . ?
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 O2 2.057(3) . ?
Co1 N4 2.055(3) . ?
Co1 O3 2.091(3) . ?
Co1 N1 2.092(3) . ?
Co1 N2 2.145(3) . ?
C1 N2 1.337(5) . ?
C1 C2 1.392(7) . ?
C2 C3 1.356(8) . ?
C3 C4 1.378(7) . ?
C4 C5 1.387(6) . ?
C5 N2 1.347(5) . ?
C5 C6 1.476(6) . ?
C6 N1 1.355(5) . ?
C6 C7 1.395(5) . ?
C7 C8 1.369(7) . ?
C8 C9 1.360(8) . ?
C9 C10 1.403(7) . ?
C10 N1 1.329(6) . ?
C11 O4 1.256(5) . ?
C11 N4 1.334(5) . ?
C11 C12 1.470(5) . ?
C12 C17 1.399(4) . ?
C12 C13 1.402(5) . ?
C13 C14 1.377(5) . ?
C14 C15 1.408(5) . ?
C14 C18 1.509(5) 1_655 ?
C15 C16 1.377(5) . ?
C16 C17 1.390(5) . ?
C17 C19 1.469(4) 2_564 ?
C18 O1 1.237(6) . ?
C18 O2 1.279(6) . ?
C18 C14 1.509(5) 1_455 ?
C19 O3 1.265(4) . ?
C19 N3 1.320(5) 2_565 ?
C19 C17 1.469(4) 2_565 ?
N3 C19 1.320(5) 2_564 ?
N3 N4 1.389(4) . ?
