#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:47:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179306 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320372.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_4320372
loop_
_publ_author_name
'Fung-E Hong'
'Yu-Tain Tsai'
Chang
'Bao-Tsan Ko'
_publ_section_title
;
 Linking Two Alkyne-Bridged Dicobalt Complexes via a Urea-Based Ligand:
 Synthesis and Spectroscopic and Structural Characterization of
 {[Co2(CO)6(μ-HC\\tbC-)]-CH2NH}2CO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5487
_journal_page_last               5488
_journal_paper_doi               10.1021/ic010071e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H5 Co3 O9'
_chemical_formula_weight         469.95
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.196(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.973(5)
_cell_length_b                   25.880(17)
_cell_length_c                   8.781(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1677.6(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.3590
_diffrn_reflns_av_sigmaI/netI    0.2753
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9597
_diffrn_reflns_theta_full        26.16
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.2101
_refine_ls_R_factor_gt           0.1050
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2830
_reflns_number_gt                1094
_reflns_number_total             3310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010071e_2.cif
_cod_data_source_block           tytu6m
_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        1677.7(19)
_cod_database_code               4320372
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.5822(2) 0.11390(6) 0.6219(2) 0.0715(8) Uani 1 1 d . . .
Co2 Co 0.9006(2) 0.08355(7) 0.7299(2) 0.0698(7) Uani 1 1 d . . .
Co3 Co 0.7734(2) 0.12580(6) 0.9131(2) 0.0696(7) Uani 1 1 d . . .
O1 O 0.3136(18) 0.1923(6) 0.582(2) 0.154(7) Uani 1 1 d . . .
O2 O 0.3897(16) 0.0177(5) 0.6396(15) 0.114(5) Uani 1 1 d . . .
O3 O 0.5529(16) 0.1182(5) 0.2823(16) 0.120(5) Uani 1 1 d . . .
O4 O 1.2801(13) 0.0982(5) 0.9365(18) 0.138(7) Uani 1 1 d . . .
O5 O 0.8366(17) -0.0255(4) 0.7860(17) 0.115(5) Uani 1 1 d . . .
O6 O 0.967(2) 0.0790(7) 0.429(2) 0.158(7) Uani 1 1 d . . .
O7 O 0.546(2) 0.2053(6) 0.969(2) 0.152(7) Uani 1 1 d . . .
O8 O 1.1053(16) 0.1562(5) 1.1851(15) 0.128(6) Uani 1 1 d . . .
O9 O 0.6872(17) 0.0321(5) 1.0567(15) 0.111(5) Uani 1 1 d . . .
C1 C 0.414(2) 0.1621(8) 0.606(2) 0.109(7) Uani 1 1 d . . .
C2 C 0.461(2) 0.0548(6) 0.6337(19) 0.095(7) Uani 1 1 d . . .
C3 C 0.575(2) 0.1160(6) 0.4056(19) 0.078(5) Uani 1 1 d . . .
C4 C 1.126(2) 0.0920(6) 0.8600(19) 0.105(7) Uani 1 1 d . . .
C5 C 0.8586(18) 0.0163(7) 0.764(2) 0.092(6) Uani 1 1 d . . .
C6 C 0.9285(17) 0.0818(7) 0.554(2) 0.083(5) Uani 1 1 d . . .
C7 C 0.629(3) 0.1737(7) 0.957(2) 0.101(7) Uani 1 1 d . . .
C8 C 0.989(3) 0.1450(6) 1.0693(19) 0.097(6) Uani 1 1 d . . .
C9 C 0.7147(18) 0.0679(6) 1.0013(19) 0.072(4) Uani 1 1 d . . .
C10 C 0.8052(17) 0.1508(5) 0.7244(17) 0.066(4) Uani 1 1 d . . .
C11 C 0.855(3) 0.2008(8) 0.682(2) 0.144(11) Uani 1 1 d . . .
H11A H 0.8838 0.1954 0.5852 0.172 Uiso 1 1 calc R . .
H11B H 0.7449 0.2214 0.6458 0.172 Uiso 1 1 calc R . .
C12 C 0.982(6) 0.2304(11) 0.779(4) 0.36(3) Uani 1 1 d . . .
H12A H 0.9832 0.2624 0.7239 0.534 Uiso 1 1 calc R . .
H12B H 1.0968 0.2135 0.8074 0.534 Uiso 1 1 calc R . .
H12C H 0.9593 0.2373 0.8769 0.534 Uiso 1 1 calc R . .
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'
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
C1 Co1 C2 101.0(9) . . ?
C1 Co1 C3 99.6(8) . . ?
C2 Co1 C3 105.5(7) . . ?
C1 Co1 C10 102.9(7) . . ?
C2 Co1 C10 143.5(5) . . ?
C3 Co1 C10 97.3(7) . . ?
C1 Co1 Co3 98.4(6) . . ?
C2 Co1 Co3 100.3(5) . . ?
C3 Co1 Co3 145.0(5) . . ?
C10 Co1 Co3 49.2(5) . . ?
C1 Co1 Co2 151.1(6) . . ?
C2 Co1 Co2 101.5(5) . . ?
C3 Co1 Co2 91.7(5) . . ?
C10 Co1 Co2 49.0(4) . . ?
Co3 Co1 Co2 59.83(8) . . ?
C6 Co2 C4 98.5(9) . . ?
C6 Co2 C5 103.1(8) . . ?
C4 Co2 C5 102.8(7) . . ?
C6 Co2 C10 101.4(8) . . ?
C4 Co2 C10 101.9(6) . . ?
C5 Co2 C10 141.9(7) . . ?
C6 Co2 Co3 149.7(6) . . ?
C4 Co2 Co3 95.4(7) . . ?
C5 Co2 Co3 99.9(6) . . ?
C10 Co2 Co3 49.2(5) . . ?
C6 Co2 Co1 97.6(5) . . ?
C4 Co2 Co1 149.9(6) . . ?
C5 Co2 Co1 98.1(4) . . ?
C10 Co2 Co1 49.8(4) . . ?
Co3 Co2 Co1 59.54(9) . . ?
C8 Co3 C9 103.0(6) . . ?
C8 Co3 C7 98.5(8) . . ?
C9 Co3 C7 100.6(9) . . ?
C8 Co3 C10 99.6(7) . . ?
C9 Co3 C10 142.7(6) . . ?
C7 Co3 C10 104.8(7) . . ?
C8 Co3 Co1 149.3(7) . . ?
C9 Co3 Co1 100.5(4) . . ?
C7 Co3 Co1 96.3(5) . . ?
C10 Co3 Co1 50.4(3) . . ?
C8 Co3 Co2 96.3(7) . . ?
C9 Co3 Co2 98.5(6) . . ?
C7 Co3 Co2 152.4(6) . . ?
C10 Co3 Co2 49.5(4) . . ?
Co1 Co3 Co2 60.63(9) . . ?
O1 C1 Co1 173(2) . . ?
O2 C2 Co1 178.2(19) . . ?
O3 C3 Co1 172.0(17) . . ?
O4 C4 Co2 175(2) . . ?
O5 C5 Co2 178.4(14) . . ?
O6 C6 Co2 173.7(14) . . ?
O7 C7 Co3 172(2) . . ?
O8 C8 Co3 167.1(19) . . ?
O9 C9 Co3 176.7(15) . . ?
C11 C10 Co3 132.6(12) . . ?
C11 C10 Co2 133.2(16) . . ?
Co3 C10 Co2 81.3(5) . . ?
C11 C10 Co1 128.4(10) . . ?
Co3 C10 Co1 80.4(6) . . ?
Co2 C10 Co1 81.2(5) . . ?
C12 C11 C10 126(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 C1 1.799(18) . ?
Co1 C2 1.831(18) . ?
Co1 C3 1.880(19) . ?
Co1 C10 1.916(12) . ?
Co1 Co3 2.452(3) . ?
Co1 Co2 2.479(3) . ?
Co2 C6 1.64(2) . ?
Co2 C4 1.742(16) . ?
Co2 C5 1.82(2) . ?
Co2 C10 1.892(13) . ?
Co2 Co3 2.459(4) . ?
Co3 C8 1.816(15) . ?
Co3 C9 1.827(17) . ?
Co3 C7 1.83(2) . ?
Co3 C10 1.882(17) . ?
O1 C1 1.080(18) . ?
O2 C2 1.128(17) . ?
O3 C3 1.03(2) . ?
O4 C4 1.167(18) . ?
O5 C5 1.124(19) . ?
O6 C6 1.25(2) . ?
O7 C7 1.08(2) . ?
O8 C8 1.126(14) . ?
O9 C9 1.107(17) . ?
C10 C11 1.45(2) . ?
C11 C12 1.30(3) . ?
