#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180118 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/16/7101642.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_7101642
loop_
_publ_author_name
'Ramírez, Juan'
'Stadler, Adrian-Mihail'
'Kyritsakas, Nathalie'
'Lehn, Jean-Marie'
_publ_section_title
;
 Solvent-modulated reversible conversion of a [2 x 2]-grid into a
 pincer-like complex.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              237
_journal_page_last               239
_journal_paper_doi               10.1039/b612222a
_journal_year                    2007
_chemical_formula_moiety         'C27 H27 Co N11, 2(Cl O4)'
_chemical_formula_sum            'C27 H27 Cl2 Co N11 O8'
_chemical_formula_weight         763.43
_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                 112.93(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.542(4)
_cell_length_b                   16.699(4)
_cell_length_c                   13.539(3)
_cell_measurement_reflns_used    4680
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.3
_cell_volume                     3236.2(14)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3679
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0685P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                2528
_reflns_number_total             3679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612222a.txt
_cod_data_source_block           st1581
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7101642
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
Co Co 0.5000 0.16137(3) 0.2500 0.02427(18) Uani 1 2 d S
N1 N 0.61392(16) 0.16738(12) 0.19976(18) 0.0292(5) Uani 1 1 d .
C1 C 0.6740(2) 0.17579(16) 0.1736(2) 0.0344(7) Uani 1 1 d .
C2 C 0.7511(3) 0.1841(2) 0.1392(4) 0.0665(12) Uani 1 1 d .
N2 N 0.58253(15) 0.26031(13) 0.36348(18) 0.0274(5) Uani 1 1 d .
C3 C 0.5981(2) 0.33481(16) 0.3377(2) 0.0346(7) Uani 1 1 d .
C4 C 0.6412(2) 0.39348(17) 0.4132(3) 0.0441(8) Uani 1 1 d .
C5 C 0.6724(2) 0.3746(2) 0.5207(3) 0.0485(9) Uani 1 1 d .
C6 C 0.6622(2) 0.29721(18) 0.5492(2) 0.0411(8) Uani 1 1 d .
C7 C 0.61729(18) 0.24185(17) 0.4691(2) 0.0299(6) Uani 1 1 d .
C8 C 0.61273(19) 0.15819(16) 0.4951(2) 0.0304(6) Uani 1 1 d .
N3 N 0.57721(15) 0.11068(12) 0.41670(17) 0.0256(5) Uani 1 1 d .
N4 N 0.57510(16) 0.03041(12) 0.43210(18) 0.0284(5) Uani 1 1 d .
C9 C 0.6240(2) -0.00599(17) 0.5368(2) 0.0338(7) Uani 1 1 d .
N5 N 0.5000 0.03023(17) 0.2500 0.0254(7) Uani 1 2 d S
C10 C 0.53533(18) -0.01297(15) 0.3393(2) 0.0267(6) Uani 1 1 d .
N6 N 0.53409(16) -0.09279(12) 0.34570(19) 0.0308(6) Uani 1 1 d .
C11 C 0.5000 -0.1292(2) 0.2500 0.0290(9) Uani 1 2 d S
C12 C 0.5000 -0.2182(2) 0.2500 0.0330(10) Uani 1 2 d S
C13 C 0.4806(2) -0.26017(17) 0.1546(3) 0.0393(8) Uani 1 1 d .
C14 C 0.4811(2) -0.34324(18) 0.1547(3) 0.0476(9) Uani 1 1 d .
C15 C 0.5000 -0.3841(2) 0.2500 0.0504(13) Uani 1 2 d S
Cl Cl 0.77616(5) 0.91933(5) 0.33185(6) 0.0433(2) Uani 1 1 d .
O1 O 0.7195(2) 0.86549(15) 0.2551(2) 0.0789(10) Uani 1 1 d .
O2 O 0.7618(3) 0.9281(3) 0.4244(2) 0.1225(16) Uani 1 1 d .
O3 O 0.8025(5) 0.9814(3) 0.2831(5) 0.0617(17) Uani 0.50 1 d P
O4 O 0.8592(4) 0.8640(4) 0.3803(4) 0.0651(15) Uani 0.50 1 d P
O5 O 0.7083(4) 0.9902(3) 0.2928(5) 0.0756(17) Uani 0.50 1 d P
O6 O 0.8611(5) 0.9480(6) 0.3327(7) 0.111(3) Uani 0.50 1 d P
H1 H 0.7674 0.2392 0.1406 0.085 Uiso 1 1 d .
H2 H 0.8035 0.1549 0.1863 0.085 Uiso 1 1 d .
H3 H 0.7331 0.1641 0.0684 0.085 Uiso 1 1 d .
H4 H 0.5791 0.3480 0.2641 0.044 Uiso 1 1 d .
H5 H 0.6493 0.4458 0.3911 0.058 Uiso 1 1 d .
H6 H 0.6995 0.4144 0.5735 0.064 Uiso 1 1 d .
H7 H 0.6852 0.2818 0.6222 0.052 Uiso 1 1 d .
H8 H 0.6363 0.1397 0.5677 0.039 Uiso 1 1 d .
H9 H 0.6142 -0.0622 0.5309 0.045 Uiso 1 1 d .
H10 H 0.6887 0.0052 0.5602 0.045 Uiso 1 1 d .
H11 H 0.6004 0.0155 0.5859 0.045 Uiso 1 1 d .
H12 H 0.4663 -0.2318 0.0894 0.052 Uiso 1 1 d .
H13 H 0.4695 -0.3721 0.0904 0.063 Uiso 1 1 d .
H14 H 0.5000 -0.4410 0.2500 0.065 Uiso 1 2 d S
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'
Cl Cl 0.1484 0.1585 '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
N1 Co N1 174.60(11) . 2_655
N1 Co N5 92.70(6) . .
N1 Co N5 92.70(6) 2_655 .
N1 Co N3 83.30(8) . 2_655
N1 Co N3 98.74(8) 2_655 2_655
N5 Co N3 68.08(5) . 2_655
N1 Co N3 98.74(8) . .
N1 Co N3 83.30(8) 2_655 .
N5 Co N3 68.08(5) . .
N3 Co N3 136.15(11) 2_655 .
N1 Co N2 82.05(8) . .
N1 Co N2 94.01(8) 2_655 .
N5 Co N2 136.43(6) . .
N3 Co N2 151.87(8) 2_655 .
N3 Co N2 70.07(8) . .
N1 Co N2 94.01(8) . 2_655
N1 Co N2 82.06(8) 2_655 2_655
N5 Co N2 136.43(6) . 2_655
N3 Co N2 70.07(8) 2_655 2_655
N3 Co N2 151.87(8) . 2_655
N2 Co N2 87.14(11) . 2_655
C1 N1 Co 175.5(2) . .
N1 C1 C2 178.3(3) . .
C1 C2 H1 109.4 . .
C1 C2 H2 109.6 . .
H1 C2 H2 109.3 . .
C1 C2 H3 109.6 . .
H1 C2 H3 109.4 . .
H2 C2 H3 109.7 . .
C3 N2 C7 116.7(2) . .
C3 N2 Co 127.5(2) . .
C7 N2 Co 115.80(17) . .
N2 C3 C4 123.4(3) . .
N2 C3 H4 118.4 . .
C4 C3 H4 118.2 . .
C5 C4 C3 119.1(3) . .
C5 C4 H5 120.6 . .
C3 C4 H5 120.3 . .
C6 C5 C4 118.6(3) . .
C6 C5 H6 121.0 . .
C4 C5 H6 120.4 . .
C5 C6 C7 119.0(3) . .
C5 C6 H7 120.7 . .
C7 C6 H7 120.3 . .
N2 C7 C6 123.1(3) . .
N2 C7 C8 116.1(2) . .
C6 C7 C8 120.6(3) . .
N3 C8 C7 116.5(2) . .
N3 C8 H8 121.8 . .
C7 C8 H8 121.7 . .
C8 N3 N4 121.2(2) . .
C8 N3 Co 119.29(18) . .
N4 N3 Co 119.08(16) . .
N3 N4 C10 114.2(2) . .
N3 N4 C9 121.8(2) . .
C10 N4 C9 123.3(2) . .
N4 C9 H9 109.0 . .
N4 C9 H10 109.1 . .
H9 C9 H10 109.8 . .
N4 C9 H11 109.1 . .
H9 C9 H11 109.7 . .
H10 C9 H11 110.0 . .
C10 N5 C10 114.3(3) 2_655 .
C10 N5 Co 122.87(15) 2_655 .
C10 N5 Co 122.87(15) . .
N5 C10 N6 126.1(3) . .
N5 C10 N4 115.2(2) . .
N6 C10 N4 118.7(2) . .
C10 N6 C11 113.6(2) . .
N6 C11 N6 126.0(3) . 2_655
N6 C11 C12 117.00(16) . .
N6 C11 C12 117.00(16) 2_655 .
C13 C12 C13 119.7(3) . 2_655
C13 C12 C11 120.16(17) . .
C13 C12 C11 120.16(17) 2_655 .
C14 C13 C12 120.2(3) . .
C14 C13 H12 119.9 . .
C12 C13 H12 119.9 . .
C15 C14 C13 119.4(3) . .
C15 C14 H13 120.0 . .
C13 C14 H13 120.6 . .
C14 C15 C14 121.1(4) 2_655 .
C14 C15 H14 119.5 2_655 .
C14 C15 H14 119.5 . .
O2 Cl O3 123.1(3) . .
O2 Cl O1 118.2(2) . .
O3 Cl O1 110.3(3) . .
O2 Cl O6 116.6(3) . .
O1 Cl O6 123.0(3) . .
O2 Cl O4 94.8(3) . .
O3 Cl O4 107.8(4) . .
O1 Cl O4 96.5(3) . .
O6 Cl O4 64.1(5) . .
O2 Cl O5 84.1(3) . .
O3 Cl O5 63.1(4) . .
O1 Cl O5 95.2(2) . .
O6 Cl O5 105.0(5) . .
O4 Cl O5 167.2(3) . .
O6 O3 Cl 68.9(6) . .
O6 O3 O5 127.9(7) . .
Cl O3 O5 63.6(3) . .
Cl O4 O6 54.4(3) . .
O3 O5 Cl 53.3(3) . .
O3 O6 Cl 66.3(5) . .
O3 O6 O4 126.3(7) . .
Cl O6 O4 61.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N1 2.132(2) .
Co N1 2.132(2) 2_655
Co N5 2.190(3) .
Co N3 2.267(2) 2_655
Co N3 2.267(2) .
Co N2 2.280(2) .
Co N2 2.280(2) 2_655
N1 C1 1.128(4) .
C1 C2 1.453(5) .
C2 H1 0.9531 .
C2 H2 0.9494 .
C2 H3 0.9483 .
N2 C3 1.339(3) .
N2 C7 1.352(3) .
C3 C4 1.385(4) .
C3 H4 0.9492 .
C4 C5 1.380(5) .
C4 H5 0.9471 .
C5 C6 1.376(5) .
C5 H6 0.9463 .
C6 C7 1.388(4) .
C6 H7 0.9470 .
C7 C8 1.449(4) .
C8 N3 1.267(3) .
C8 H8 0.9554 .
N3 N4 1.359(3) .
N4 C10 1.371(3) .
N4 C9 1.455(3) .
C9 H9 0.9495 .
C9 H10 0.9466 .
C9 H11 0.9474 .
N5 C10 1.329(3) 2_655
N5 C10 1.329(3) .
C10 N6 1.336(3) .
N6 C11 1.339(3) .
C11 N6 1.340(3) 2_655
C11 C12 1.486(5) .
C12 C13 1.395(4) .
C12 C13 1.395(4) 2_655
C13 C14 1.387(4) .
C13 H12 0.9494 .
C14 C15 1.386(4) .
C14 H13 0.9486 .
C15 C14 1.386(4) 2_655
C15 H14 0.9498 .
Cl O2 1.363(3) .
Cl O3 1.374(5) .
Cl O1 1.397(2) .
Cl O6 1.400(7) .
Cl O4 1.514(5) .
Cl O5 1.535(5) .
O3 O6 1.056(9) .
O3 O5 1.527(9) .
O4 O6 1.548(11) .
