#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:08:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179502 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/99/4339937.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_4339937
loop_
_publ_author_name
'Barrios, Leoní A'
'Ribas, Joan'
'Aromí, Guillem'
'Ribas-Ariño, Jordi'
'Gamez, Patrick'
'Roubeau, Olivier'
'Teat, Simon J.'
_publ_section_title
;
 Preparation and structure of three solvatomorphs of the polymer
 [Co(dbm)2(4ptz)]n: spin canting depending on the supramolecular
 organization.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7154
_journal_page_last               7162
_journal_paper_doi               10.1021/ic7004979
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C32 H30 Co O6'
_chemical_formula_weight         569.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.779(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9583(8)
_cell_length_b                   16.3460(7)
_cell_length_c                   10.3880(6)
_cell_measurement_reflns_used    14261
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2726.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11634
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0410
_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)+(0.0542P)²+2.3071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                2956
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7004979-file002.cif
_cod_data_source_block           ga488b
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4339937
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'
'-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
Co1 Co 0.5000 0.01622(2) 0.2500 0.01682(11) Uani 1 2 d S
O1 O 0.46484(8) 0.10495(8) 0.36127(13) 0.0202(3) Uani 1 1 d .
O2 O 0.38396(8) 0.01922(8) 0.11298(13) 0.0208(3) Uani 1 1 d .
O3 O 0.46461(8) -0.07840(8) 0.35880(13) 0.0246(3) Uani 1 1 d .
H3 H 0.4878 -0.0930 0.4397 0.037 Uiso 1 1 calc R
C1 C 0.40477(11) 0.15511(11) 0.30883(18) 0.0191(3) Uani 1 1 d .
C2 C 0.33315(10) 0.07825(11) 0.09508(18) 0.0186(3) Uani 1 1 d .
C3 C 0.34327(11) 0.14677(11) 0.18265(19) 0.0216(4) Uani 1 1 d .
H3A H 0.3050 0.1906 0.1529 0.026 Uiso 1 1 calc R
C4 C 0.40309(12) 0.22826(11) 0.39391(19) 0.0214(4) Uani 1 1 d .
C5 C 0.32921(13) 0.26312(12) 0.4010(2) 0.0285(4) Uani 1 1 d .
H5A H 0.2770 0.2410 0.3481 0.034 Uiso 1 1 calc R
C6 C 0.33186(15) 0.32977(14) 0.4848(2) 0.0354(5) Uani 1 1 d .
H6A H 0.2815 0.3528 0.4898 0.043 Uiso 1 1 calc R
C7 C 0.40779(16) 0.36304(13) 0.5615(2) 0.0362(5) Uani 1 1 d .
H7A H 0.4093 0.4086 0.6190 0.043 Uiso 1 1 calc R
C8 C 0.48116(15) 0.32982(12) 0.5543(2) 0.0328(5) Uani 1 1 d .
H8A H 0.5331 0.3530 0.6060 0.039 Uiso 1 1 calc R
C9 C 0.47917(12) 0.26268(12) 0.4717(2) 0.0254(4) Uani 1 1 d .
H9A H 0.5299 0.2398 0.4678 0.031 Uiso 1 1 calc R
C10 C 0.25715(10) 0.07181(11) -0.02845(18) 0.0190(4) Uani 1 1 d .
C11 C 0.18586(11) 0.11945(12) -0.0474(2) 0.0242(4) Uani 1 1 d .
H11A H 0.1855 0.1602 0.0176 0.029 Uiso 1 1 calc R
C12 C 0.11564(12) 0.10783(13) -0.1600(2) 0.0275(4) Uani 1 1 d .
H12A H 0.0674 0.1403 -0.1714 0.033 Uiso 1 1 calc R
C13 C 0.11574(11) 0.04899(13) -0.2556(2) 0.0267(4) Uani 1 1 d .
H13A H 0.0674 0.0404 -0.3320 0.032 Uiso 1 1 calc R
C14 C 0.18688(12) 0.00246(13) -0.2397(2) 0.0276(4) Uani 1 1 d .
H14A H 0.1876 -0.0370 -0.3065 0.033 Uiso 1 1 calc R
C15 C 0.25683(11) 0.01350(12) -0.1264(2) 0.0232(4) Uani 1 1 d .
H15A H 0.3050 -0.0190 -0.1155 0.028 Uiso 1 1 calc R
C16 C 0.40398(12) -0.13797(12) 0.2906(2) 0.0270(4) Uani 1 1 d .
H16A H 0.3958 -0.1767 0.3572 0.040 Uiso 1 1 calc R
H16B H 0.4234 -0.1675 0.2243 0.040 Uiso 1 1 calc R
H16C H 0.3511 -0.1106 0.2435 0.040 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
O2 Co1 O2 177.22(7) . 2_655
O2 Co1 O1 89.20(5) . .
O2 Co1 O1 88.85(5) 2_655 .
O2 Co1 O1 88.85(5) . 2_655
O2 Co1 O1 89.20(5) 2_655 2_655
O1 Co1 O1 90.43(7) . 2_655
O2 Co1 O3 91.19(5) . 2_655
O2 Co1 O3 90.84(5) 2_655 2_655
O1 Co1 O3 177.72(5) . 2_655
O1 Co1 O3 91.83(5) 2_655 2_655
O2 Co1 O3 90.84(5) . .
O2 Co1 O3 91.19(5) 2_655 .
O1 Co1 O3 91.83(5) . .
O1 Co1 O3 177.72(5) 2_655 .
O3 Co1 O3 85.92(8) 2_655 .
C1 O1 Co1 123.03(11) . .
C2 O2 Co1 125.66(12) . .
C16 O3 Co1 121.12(12) . .
C16 O3 H3 109.5 . .
Co1 O3 H3 128.4 . .
O1 C1 C3 125.97(16) . .
O1 C1 C4 115.09(15) . .
C3 C1 C4 118.94(16) . .
O2 C2 C3 124.84(16) . .
O2 C2 C10 115.35(16) . .
C3 C2 C10 119.81(16) . .
C1 C3 C2 125.44(17) . .
C1 C3 H3A 117.3 . .
C2 C3 H3A 117.3 . .
C9 C4 C5 118.69(18) . .
C9 C4 C1 118.27(16) . .
C5 C4 C1 123.04(17) . .
C6 C5 C4 120.3(2) . .
C6 C5 H5A 119.9 . .
C4 C5 H5A 119.9 . .
C5 C6 C7 120.3(2) . .
C5 C6 H6A 119.8 . .
C7 C6 H6A 119.8 . .
C8 C7 C6 120.0(2) . .
C8 C7 H7A 120.0 . .
C6 C7 H7A 120.0 . .
C7 C8 C9 120.1(2) . .
C7 C8 H8A 119.9 . .
C9 C8 H8A 119.9 . .
C8 C9 C4 120.60(19) . .
C8 C9 H9A 119.7 . .
C4 C9 H9A 119.7 . .
C15 C10 C11 118.61(17) . .
C15 C10 C2 118.21(16) . .
C11 C10 C2 123.14(17) . .
C12 C11 C10 120.72(18) . .
C12 C11 H11A 119.6 . .
C10 C11 H11A 119.6 . .
C13 C12 C11 120.11(18) . .
C13 C12 H12A 119.9 . .
C11 C12 H12A 119.9 . .
C12 C13 C14 119.76(18) . .
C12 C13 H13A 120.1 . .
C14 C13 H13A 120.1 . .
C15 C14 C13 120.14(19) . .
C15 C14 H14A 119.9 . .
C13 C14 H14A 119.9 . .
C14 C15 C10 120.64(18) . .
C14 C15 H15A 119.7 . .
C10 C15 H15A 119.7 . .
O3 C16 H16A 109.5 . .
O3 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O3 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.0242(12) .
Co1 O2 2.0242(12) 2_655
Co1 O1 2.0589(13) .
Co1 O1 2.0589(13) 2_655
Co1 O3 2.1134(13) 2_655
Co1 O3 2.1134(13) .
O1 C1 1.284(2) .
O2 C2 1.267(2) .
O3 C16 1.428(2) .
O3 H3 0.8400 .
C1 C3 1.394(3) .
C1 C4 1.493(3) .
C2 C3 1.418(3) .
C2 C10 1.501(2) .
C3 H3A 0.9500 .
C4 C9 1.401(3) .
C4 C5 1.400(3) .
C5 C6 1.386(3) .
C5 H5A 0.9500 .
C6 C7 1.389(3) .
C6 H6A 0.9500 .
C7 C8 1.382(3) .
C7 H7A 0.9500 .
C8 C9 1.387(3) .
C8 H8A 0.9500 .
C9 H9A 0.9500 .
C10 C15 1.393(3) .
C10 C11 1.398(2) .
C11 C12 1.388(3) .
C11 H11A 0.9500 .
C12 C13 1.383(3) .
C12 H12A 0.9500 .
C13 C14 1.390(3) .
C13 H13A 0.9500 .
C14 C15 1.388(3) .
C14 H14A 0.9500 .
C15 H15A 0.9500 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
