#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:40:04 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180150 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/47/7104747.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_7104747
loop_
_publ_author_name
'Duriska, Martin B'
'Neville, Suzanne M'
'Batten, Stuart R'
_publ_section_title
;
 Variable length ligands: a new class of bridging ligands for
 supramolecular chemistry and crystal engineering.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5579
_journal_page_last               5581
_journal_paper_doi               10.1039/b910994c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C24 H40 Cl2 Co K N4 O6, 2(H2 O), (Cl)'
_chemical_formula_sum            'C24 H44 Cl3 Co K N4 O8'
_chemical_formula_weight         721.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '9 November 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.956(1)
_cell_angle_beta                 112.965(1)
_cell_angle_gamma                101.559(1)
_cell_formula_units_Z            1
_cell_length_a                   9.4628(1)
_cell_length_b                   9.9583(1)
_cell_length_c                   10.5733(2)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.81
_cell_measurement_theta_min      2.42
_cell_volume                     834.01(2)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'MERCURY 1.4 (Bruno et al., 2002)'
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  X-SEED
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15460
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.8929
_exptl_absorpt_correction_T_min  0.7525
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             377
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.253
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0505
_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)+(0.0739P)²+1.7946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                4300
_reflns_number_total             5014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910994c.txt
_cod_data_source_block           G
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104747
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.0000 0.0000 0.01227(12) Uani 1 2 d S . .
K1 K 1.5000 0.5000 1.0000 0.01486(15) Uani 1 2 d S . .
Cl1 Cl 0.39939(8) -0.22001(6) 0.04452(6) 0.01835(14) Uani 1 1 d . . .
O1 O 1.1931(2) 0.4134(2) 0.9925(2) 0.0186(4) Uani 1 1 d . . .
N1 N 1.2006(3) 0.4049(2) 0.7152(2) 0.0149(4) Uani 1 1 d . . .
C1 C 1.1766(3) 0.3448(3) 1.0907(3) 0.0188(5) Uani 1 1 d . . .
H1A H 1.1689 0.2403 1.0531 0.023 Uiso 1 1 calc R . .
H1B H 1.0760 0.3475 1.0981 0.023 Uiso 1 1 calc R . .
Cl2 Cl 0.36808(15) 0.11968(14) 0.38995(14) 0.0188(2) Uani 0.50 1 d P . .
O2 O 1.5317(2) 0.5759(2) 0.77200(19) 0.0157(3) Uani 1 1 d . . .
N2 N 0.7215(3) 0.0734(2) 0.2052(2) 0.0152(4) Uani 1 1 d . . .
C2 C 1.0475(3) 0.3571(3) 0.8559(3) 0.0192(5) Uani 1 1 d . . .
H2A H 0.9566 0.3757 0.8734 0.023 Uiso 1 1 calc R . .
H2B H 1.0189 0.2492 0.8082 0.023 Uiso 1 1 calc R . .
O3 O 0.3932(2) 0.1150(2) 0.1109(2) 0.0176(3) Uani 1 1 d D . .
C3 C 1.0741(3) 0.4329(3) 0.7561(3) 0.0182(5) Uani 1 1 d . . .
H3A H 0.9699 0.3998 0.6644 0.022 Uiso 1 1 calc R . .
H3B H 1.1047 0.5407 0.8064 0.022 Uiso 1 1 calc R . .
O4A O 1.6138(8) 0.2014(6) 0.6520(6) 0.0291(11) Uani 0.50 1 d PD A 1
C4 C 1.2389(3) 0.5066(3) 0.6447(3) 0.0180(5) Uani 1 1 d . . .
H4A H 1.2506 0.6070 0.7037 0.022 Uiso 1 1 calc R . .
H4B H 1.1457 0.4759 0.5452 0.022 Uiso 1 1 calc R . .
C5 C 1.3922(3) 0.5141(3) 0.6287(3) 0.0187(5) Uani 1 1 d . . .
H5A H 1.3853 0.4137 0.5748 0.022 Uiso 1 1 calc R . .
H5B H 1.4028 0.5759 0.5709 0.022 Uiso 1 1 calc R . .
C6 C 1.6771(3) 0.5735(3) 0.7598(3) 0.0187(5) Uani 1 1 d . . .
H6A H 1.6858 0.6204 0.6900 0.022 Uiso 1 1 calc R . .
H6B H 1.6722 0.4700 0.7208 0.022 Uiso 1 1 calc R . .
C7 C 1.1609(3) 0.2473(3) 0.6269(3) 0.0154(4) Uani 1 1 d . . .
H7A H 1.1486 0.1878 0.6863 0.019 Uiso 1 1 calc R . .
H7B H 1.2542 0.2371 0.6092 0.019 Uiso 1 1 calc R . .
C8 C 1.0074(3) 0.1832(3) 0.4785(3) 0.0149(4) Uani 1 1 d . . .
C9 C 0.8547(3) 0.1252(3) 0.4667(3) 0.0177(5) Uani 1 1 d . . .
H9 H 0.8447 0.1221 0.5520 0.021 Uiso 1 1 calc R . .
C10 C 0.7163(3) 0.0718(3) 0.3301(3) 0.0175(5) Uani 1 1 d . . .
H10 H 0.6131 0.0322 0.3247 0.021 Uiso 1 1 calc R . .
C11 C 0.8691(3) 0.1265(3) 0.2158(3) 0.0200(5) Uani 1 1 d . . .
H11 H 0.8756 0.1271 0.1285 0.024 Uiso 1 1 calc R . .
C12 C 1.0129(3) 0.1808(3) 0.3479(3) 0.0203(5) Uani 1 1 d . . .
H12 H 1.1148 0.2161 0.3494 0.024 Uiso 1 1 calc R . .
O4B O 1.6778(6) 0.1773(7) 0.6853(6) 0.0322(12) Uani 0.50 1 d PD B 2
HO3A H 0.374(5) 0.117(4) 0.187(3) 0.039 Uiso 1 1 d D . .
HO3B H 0.408(5) 0.212(2) 0.135(4) 0.039 Uiso 1 1 d D . .
HO4A H 1.639(4) 0.218(4) 0.752(2) 0.039 Uiso 1 1 d D . .
HO4B H 1.581(3) 0.102(2) 0.648(4) 0.039 Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O3 Co1 O3 180.00(8) 2_655 . ?
O3 Co1 N2 90.45(8) 2_655 2_655 ?
O3 Co1 N2 89.55(8) . 2_655 ?
O3 Co1 N2 89.55(8) 2_655 . ?
O3 Co1 N2 90.45(8) . . ?
N2 Co1 N2 180.00(11) 2_655 . ?
O3 Co1 Cl1 90.84(5) 2_655 2_655 ?
O3 Co1 Cl1 89.16(5) . 2_655 ?
N2 Co1 Cl1 89.54(6) 2_655 2_655 ?
N2 Co1 Cl1 90.46(6) . 2_655 ?
O3 Co1 Cl1 89.16(5) 2_655 . ?
O3 Co1 Cl1 90.84(5) . . ?
N2 Co1 Cl1 90.46(6) 2_655 . ?
N2 Co1 Cl1 89.54(6) . . ?
Cl1 Co1 Cl1 180.00(2) 2_655 . ?
O2 K1 O2 180.000(1) 2_867 . ?
O2 K1 O1 58.98(5) 2_867 . ?
O2 K1 O1 121.02(5) . . ?
O2 K1 O1 121.02(5) 2_867 2_867 ?
O2 K1 O1 58.98(5) . 2_867 ?
O1 K1 O1 180.0 . 2_867 ?
O2 K1 N1 117.65(6) 2_867 . ?
O2 K1 N1 62.35(5) . . ?
O1 K1 N1 61.01(5) . . ?
O1 K1 N1 118.99(5) 2_867 . ?
O2 K1 N1 62.35(5) 2_867 2_867 ?
O2 K1 N1 117.65(5) . 2_867 ?
O1 K1 N1 118.99(5) . 2_867 ?
O1 K1 N1 61.01(5) 2_867 2_867 ?
N1 K1 N1 180.000(1) . 2_867 ?
O2 K1 Cl1 98.94(4) 2_867 1_666 ?
O2 K1 Cl1 81.06(4) . 1_666 ?
O1 K1 Cl1 73.79(4) . 1_666 ?
O1 K1 Cl1 106.21(4) 2_867 1_666 ?
N1 K1 Cl1 79.20(4) . 1_666 ?
N1 K1 Cl1 100.80(4) 2_867 1_666 ?
O2 K1 Cl1 81.06(4) 2_867 2_756 ?
O2 K1 Cl1 98.94(4) . 2_756 ?
O1 K1 Cl1 106.21(4) . 2_756 ?
O1 K1 Cl1 73.79(4) 2_867 2_756 ?
N1 K1 Cl1 100.80(4) . 2_756 ?
N1 K1 Cl1 79.20(4) 2_867 2_756 ?
Cl1 K1 Cl1 180.0 1_666 2_756 ?
Co1 Cl1 K1 127.22(2) . 1_444 ?
C2 O1 C1 111.6(2) . . ?
C2 O1 K1 120.29(14) . . ?
C1 O1 K1 118.71(14) . . ?
C4 N1 C3 109.3(2) . . ?
C4 N1 C7 113.54(19) . . ?
C3 N1 C7 113.6(2) . . ?
C4 N1 K1 104.71(14) . . ?
C3 N1 K1 105.29(14) . . ?
C7 N1 K1 109.61(13) . . ?
O1 C1 C6 108.6(2) . 2_867 ?
O1 C1 H1A 110.0 . . ?
C6 C1 H1A 110.0 2_867 . ?
O1 C1 H1B 110.0 . . ?
C6 C1 H1B 110.0 2_867 . ?
H1A C1 H1B 108.4 . . ?
C5 O2 C6 110.69(19) . . ?
C5 O2 K1 117.82(14) . . ?
C6 O2 K1 116.82(14) . . ?
C11 N2 C10 117.0(2) . . ?
C11 N2 Co1 122.17(17) . . ?
C10 N2 Co1 120.79(16) . . ?
O1 C2 C3 108.9(2) . . ?
O1 C2 H2A 109.9 . . ?
C3 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C3 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
Co1 O3 HO3A 136(2) . . ?
Co1 O3 HO3B 126(2) . . ?
HO3A O3 HO3B 90(2) . . ?
N1 C3 C2 114.4(2) . . ?
N1 C3 H3A 108.7 . . ?
C2 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
HO4A O4A HO4B 78.4(18) . . ?
N1 C4 C5 114.7(2) . . ?
N1 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
N1 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
O2 C5 C4 109.8(2) . . ?
O2 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
O2 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O2 C6 C1 109.6(2) . 2_867 ?
O2 C6 H6A 109.8 . . ?
C1 C6 H6A 109.8 2_867 . ?
O2 C6 H6B 109.8 . . ?
C1 C6 H6B 109.8 2_867 . ?
H6A C6 H6B 108.2 . . ?
N1 C7 C8 115.11(19) . . ?
N1 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C12 116.8(2) . . ?
C9 C8 C7 121.4(2) . . ?
C12 C8 C7 121.8(2) . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 123.1(2) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 123.3(2) . . ?
N2 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C8 119.8(2) . . ?
C11 C12 H12 120.1 . . ?
C8 C12 H12 120.1 . . ?
HO4A O4B HO4B 80.4(18) . . ?
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 O3 2.0979(18) 2_655 ?
Co1 O3 2.0979(18) . ?
Co1 N2 2.158(2) 2_655 ?
Co1 N2 2.158(2) . ?
Co1 Cl1 2.4442(6) 2_655 ?
Co1 Cl1 2.4442(6) . ?
K1 O2 2.8084(17) 2_867 ?
K1 O2 2.8084(17) . ?
K1 O1 2.8219(18) . ?
K1 O1 2.8219(18) 2_867 ?
K1 N1 2.964(2) . ?
K1 N1 2.964(2) 2_867 ?
K1 Cl1 3.1046(6) 1_666 ?
K1 Cl1 3.1046(6) 2_756 ?
Cl1 K1 3.1046(6) 1_444 ?
O1 C2 1.421(3) . ?
O1 C1 1.421(3) . ?
N1 C4 1.473(3) . ?
N1 C3 1.473(3) . ?
N1 C7 1.486(3) . ?
C1 C6 1.502(4) 2_867 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
O2 C5 1.432(3) . ?
O2 C6 1.435(3) . ?
N2 C11 1.339(3) . ?
N2 C10 1.345(3) . ?
C2 C3 1.513(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 HO3A 0.886(18) . ?
O3 HO3B 0.898(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O4A HO4A 0.953(17) . ?
O4A HO4B 0.961(17) . ?
C4 C5 1.514(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C1 1.502(4) 2_867 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.521(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.388(3) . ?
C8 C12 1.396(3) . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
O4B HO4A 0.956(17) . ?
O4B HO4B 0.918(18) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 HO3A Cl2 0.886(18) 2.164(19) 3.041(2) 170(4) .
O3 HO3B O2 0.898(18) 1.94(2) 2.826(3) 169(4) 2_766
