#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:31:35 +0100 (vie 25 de mar de 2016) $
#$Revision: 180083 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/29/7052986.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_7052986
loop_
_publ_author_name
'Jacobs, Tia'
'Barbour, Leonard J.'
_publ_section_title
;
 Single-crystal to single-crystal transformations in discrete solvated
 metallocycles: the role of the metal ion
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              71
_journal_paper_doi               10.1039/c2nj40612h
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C44 H44 Cl4 Co2 N8'
_chemical_formula_sum            'C44 H44 Cl4 Co2 N8'
_chemical_formula_weight         944.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_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                 118.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.020(4)
_cell_length_b                   14.595(3)
_cell_length_c                   17.102(3)
_cell_measurement_reflns_used    764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.96
_cell_measurement_theta_min      2.31
_cell_volume                     4386.5(19)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
X-Seed (Barbour, 2001; Atwood & Barbour, 2003)
;
_computing_publication_material
;
X-Seed (Atwood & Barbour, 2003; Barbour, 2001)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_sigmaI/netI    0.1597
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13411
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.8940
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1992
_refine_ls_R_factor_gt           0.1308
_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)+(0.0828P)²+29.6084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2320
_refine_ls_wR_factor_ref         0.2617
_reflns_number_gt                3069
_reflns_number_total             5107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40612h.txt
_cod_data_source_block           CoCl2_empty
_cod_original_cell_volume        4386.6(15)
_cod_database_code               7052986
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
Cl2 Cl 0.36765(12) 0.50840(15) 0.52958(17) 0.0363(6) Uani 1 1 d .
Cl3 Cl 0.17674(13) 0.49395(14) 0.32936(14) 0.0311(5) Uani 1 1 d .
Co1 Co 0.24219(6) 0.49232(7) 0.47957(8) 0.0198(3) Uani 1 1 d .
N4A N 0.2130(4) 0.3778(5) 0.5210(5) 0.0241(16) Uani 1 1 d .
N4B N 0.2098(4) 0.6012(5) 0.5248(5) 0.0251(17) Uani 1 1 d .
C5A C 0.1633(4) 0.3109(5) 0.4636(5) 0.0192(17) Uani 1 1 d .
H5A H 0.1374 0.3138 0.4004 0.023 Uiso 1 1 calc R
C5B C 0.2569(5) 0.6706(6) 0.5786(5) 0.0206(18) Uani 1 1 d .
H5B H 0.3109 0.6689 0.6107 0.025 Uiso 1 1 calc R
C6A C 0.1586(4) 0.2429(5) 0.5125(5) 0.0184(17) Uani 1 1 d U
H6A H 0.1291 0.1887 0.4908 0.022 Uiso 1 1 calc R
C6B C 0.2122(5) 0.7412(6) 0.5775(6) 0.025(2) Uani 1 1 d .
H6B H 0.2291 0.7978 0.6081 0.030 Uiso 1 1 calc R
N7A N 0.2051(3) 0.2659(4) 0.6015(5) 0.0179(15) Uani 1 1 d .
N7B N 0.1373(4) 0.7151(5) 0.5232(4) 0.0217(15) Uani 1 1 d .
C8A C 0.2364(4) 0.3485(5) 0.6024(6) 0.0205(18) Uani 1 1 d .
C8B C 0.1384(5) 0.6304(5) 0.4926(5) 0.0195(18) Uani 1 1 d .
C9A C 0.2907(5) 0.3969(6) 0.6839(6) 0.032(2) Uani 1 1 d .
H9A1 H 0.3137 0.4479 0.6679 0.047 Uiso 1 1 calc R
H9A2 H 0.3306 0.3544 0.7231 0.047 Uiso 1 1 calc R
H9A3 H 0.2639 0.4207 0.7148 0.047 Uiso 1 1 calc R
C9B C 0.0688(4) 0.5739(6) 0.4389(6) 0.026(2) Uani 1 1 d .
H9B1 H 0.0793 0.5294 0.4032 0.039 Uiso 1 1 calc R
H9B2 H 0.0268 0.6139 0.3993 0.039 Uiso 1 1 calc R
H9B3 H 0.0547 0.5413 0.4789 0.039 Uiso 1 1 calc R
C10A C 0.2160(5) 0.2061(5) 0.6744(6) 0.0213(18) Uani 1 1 d .
H10A H 0.2620 0.2257 0.7291 0.026 Uiso 1 1 calc R
H10B H 0.2245 0.1427 0.6605 0.026 Uiso 1 1 calc R
C10B C 0.0723(5) 0.7717(5) 0.5061(5) 0.0229(19) Uani 1 1 d .
H10C H 0.0273 0.7492 0.4519 0.028 Uiso 1 1 calc R
H10D H 0.0824 0.8354 0.4947 0.028 Uiso 1 1 calc R
C11A C 0.1481(5) 0.2071(6) 0.6915(5) 0.0216(18) Uani 1 1 d .
C11B C 0.0553(4) 0.7712(5) 0.5819(5) 0.0186(18) Uani 1 1 d .
C12A C 0.1066(4) 0.1270(5) 0.6818(5) 0.0186(17) Uani 1 1 d .
H12A H 0.1176 0.0730 0.6591 0.022 Uiso 1 1 calc R
C12B C 0.0658(4) 0.6957(6) 0.6342(5) 0.0216(18) Uani 1 1 d .
H12B H 0.0883 0.6424 0.6248 0.026 Uiso 1 1 calc R
C13A C 0.0497(4) 0.1267(5) 0.7055(5) 0.0139(16) Uani 1 1 d .
H13A H 0.0223 0.0716 0.6992 0.017 Uiso 1 1 calc R
C13B C 0.0446(4) 0.6945(5) 0.7004(5) 0.0196(18) Uani 1 1 d .
H13B H 0.0529 0.6411 0.7357 0.024 Uiso 1 1 calc R
C14A C 0.0312(4) 0.2039(5) 0.7381(5) 0.0121(15) Uani 1 1 d U
C14B C 0.0113(4) 0.7710(6) 0.7151(5) 0.0199(18) Uani 1 1 d .
C15A C 0.0730(4) 0.2840(5) 0.7456(5) 0.0155(16) Uani 1 1 d .
H15A H 0.0612 0.3388 0.7663 0.019 Uiso 1 1 calc R
C15B C 0.0038(4) 0.8487(5) 0.6646(5) 0.0198(18) Uani 1 1 d .
H15B H -0.0162 0.9030 0.6761 0.024 Uiso 1 1 calc R
C16A C 0.1302(4) 0.2845(5) 0.7235(5) 0.0206(18) Uani 1 1 d .
H16A H 0.1581 0.3393 0.7305 0.025 Uiso 1 1 calc R
C16B C 0.0242(4) 0.8500(5) 0.5990(5) 0.0190(17) Uani 1 1 d .
H16B H 0.0174 0.9041 0.5651 0.023 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'
N N 0.0061 0.0033 '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'
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_3
N4B Co1 N4A 108.7(3) .
N4B Co1 Cl2 106.2(2) .
N4A Co1 Cl2 114.5(2) .
N4B Co1 Cl3 108.2(2) .
N4A Co1 Cl3 107.6(2) .
Cl2 Co1 Cl3 111.49(11) .
C8A N4A C5A 106.8(7) .
C8A N4A Co1 129.1(6) .
C5A N4A Co1 124.1(6) .
C8B N4B C5B 107.1(7) .
C8B N4B Co1 125.1(6) .
C5B N4B Co1 126.2(5) .
C6A C5A N4A 108.6(7) .
C6A C5A H5A 125.7 .
N4A C5A H5A 125.7 .
C6B C5B N4B 108.0(7) .
C6B C5B H5B 126.0 .
N4B C5B H5B 126.0 .
C5A C6A N7A 107.2(7) .
C5A C6A H6A 126.4 .
N7A C6A H6A 126.4 .
C5B C6B N7B 107.1(8) .
C5B C6B H6B 126.4 .
N7B C6B H6B 126.4 .
C8A N7A C6A 106.9(7) .
C8A N7A C10A 130.3(7) .
C6A N7A C10A 122.8(7) .
C8B N7B C6B 107.5(7) .
C8B N7B C10B 128.7(7) .
C6B N7B C10B 123.8(7) .
N4A C8A N7A 110.5(7) .
N4A C8A C9A 125.1(8) .
N7A C8A C9A 124.4(8) .
N4B C8B N7B 110.3(7) .
N4B C8B C9B 125.2(7) .
N7B C8B C9B 124.2(7) .
C8A C9A H9A1 109.5 .
C8A C9A H9A2 109.5 .
H9A1 C9A H9A2 109.5 .
C8A C9A H9A3 109.5 .
H9A1 C9A H9A3 109.5 .
H9A2 C9A H9A3 109.5 .
C8B C9B H9B1 109.5 .
C8B C9B H9B2 109.5 .
H9B1 C9B H9B2 109.5 .
C8B C9B H9B3 109.5 .
H9B1 C9B H9B3 109.5 .
H9B2 C9B H9B3 109.5 .
N7A C10A C11A 112.3(6) .
N7A C10A H10A 109.1 .
C11A C10A H10A 109.1 .
N7A C10A H10B 109.1 .
C11A C10A H10B 109.1 .
H10A C10A H10B 107.9 .
N7B C10B C11B 112.3(7) .
N7B C10B H10C 109.1 .
C11B C10B H10C 109.1 .
N7B C10B H10D 109.1 .
C11B C10B H10D 109.1 .
H10C C10B H10D 107.9 .
C16A C11A C12A 118.7(8) .
C16A C11A C10A 120.7(7) .
C12A C11A C10A 120.3(7) .
C12B C11B C16B 117.8(8) .
C12B C11B C10B 123.0(7) .
C16B C11B C10B 119.2(7) .
C13A C12A C11A 119.7(7) .
C13A C12A H12A 120.1 .
C11A C12A H12A 120.1 .
C11B C12B C13B 122.2(8) .
C11B C12B H12B 118.9 .
C13B C12B H12B 118.9 .
C12A C13A C14A 122.2(7) .
C12A C13A H13A 118.9 .
C14A C13A H13A 118.9 .
C14B C13B C12B 120.1(7) .
C14B C13B H13B 120.0 .
C12B C13B H13B 120.0 .
C13A C14A C15A 116.8(7) .
C13A C14A C14A 122.1(5) 2_556
C15A C14A C14A 121.1(5) 2_556
C13B C14B C15B 117.6(8) .
C13B C14B C14B 120.8(6) 2_556
C15B C14B C14B 121.5(5) 2_556
C16A C15A C14A 121.4(7) .
C16A C15A H15A 119.3 .
C14A C15A H15A 119.3 .
C16B C15B C14B 122.4(8) .
C16B C15B H15B 118.8 .
C14B C15B H15B 118.8 .
C15A C16A C11A 121.2(8) .
C15A C16A H16A 119.4 .
C11A C16A H16A 119.4 .
C15B C16B C11B 119.9(7) .
C15B C16B H16B 120.1 .
C11B C16B H16B 120.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl2 Co1 2.244(2) .
Cl3 Co1 2.256(3) .
Co1 N4B 2.006(7) .
Co1 N4A 2.008(7) .
N4A C8A 1.310(10) .
N4A C5A 1.404(10) .
N4B C8B 1.332(10) .
N4B C5B 1.390(11) .
C5A C6A 1.331(11) .
C5A H5A 0.9500 .
C5B C6B 1.359(11) .
C5B H5B 0.9500 .
C6A N7A 1.392(10) .
C6A H6A 0.9500 .
C6B N7B 1.386(11) .
C6B H6B 0.9500 .
N7A C8A 1.356(10) .
N7A C10A 1.449(10) .
N7B C8B 1.345(10) .
N7B C10B 1.448(10) .
C8A C9A 1.473(11) .
C8B C9B 1.497(11) .
C9A H9A1 0.9800 .
C9A H9A2 0.9800 .
C9A H9A3 0.9800 .
C9B H9B1 0.9800 .
C9B H9B2 0.9800 .
C9B H9B3 0.9800 .
C10A C11A 1.521(11) .
C10A H10A 0.9900 .
C10A H10B 0.9900 .
C10B C11B 1.489(11) .
C10B H10C 0.9900 .
C10B H10D 0.9900 .
C11A C16A 1.377(11) .
C11A C12A 1.397(11) .
C11B C12B 1.372(11) .
C11B C16B 1.403(10) .
C12A C13A 1.379(11) .
C12A H12A 0.9500 .
C12B C13B 1.385(11) .
C12B H12B 0.9500 .
C13A C14A 1.386(10) .
C13A H13A 0.9500 .
C13B C14B 1.385(11) .
C13B H13B 0.9500 .
C14A C15A 1.406(10) .
C14A C14A 1.487(14) 2_556
C14B C15B 1.390(11) .
C14B C14B 1.465(16) 2_556
C15A C16A 1.366(11) .
C15A H15A 0.9500 .
C15B C16B 1.365(11) .
C15B H15B 0.9500 .
C16A H16A 0.9500 .
C16B H16B 0.9500 .
