#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:31:35 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180083 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/29/7052985.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_7052985
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, 2(C H4 O)'
_chemical_formula_sum            'C46 H52 Cl4 Co2 N8 O2'
_chemical_formula_weight         1008.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 114.150(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.232(2)
_cell_length_b                   15.471(2)
_cell_length_c                   9.4730(11)
_cell_measurement_reflns_used    729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.23
_cell_measurement_theta_min      2.36
_cell_volume                     2304.4(5)
_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 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7310
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.8980
_exptl_absorpt_correction_T_min  0.7536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0826
_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)+(0.0704P)²+3.5943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                2072
_reflns_number_total             2774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40612h.txt
_cod_data_source_block           CoCl2_MeOH
_cod_original_cell_volume        2304.3(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7052985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Cl2 Cl 0.13008(11) 0.0000 0.9916(2) 0.0256(4) Uani 1 2 d S
Cl3 Cl 0.34413(14) 0.0000 1.3445(2) 0.0342(5) Uani 1 2 d S
Co1 Co 0.27408(6) 0.0000 1.08151(10) 0.0161(3) Uani 1 2 d S
N4 N 0.3138(2) 0.1095(2) 1.0198(4) 0.0160(8) Uani 1 1 d .
C5 C 0.3841(3) 0.1565(3) 1.1162(6) 0.0241(11) Uani 1 1 d .
H5 H 0.4218 0.1399 1.2178 0.029 Uiso 1 1 calc R
C6 C 0.3907(3) 0.2288(3) 1.0439(6) 0.0244(11) Uani 1 1 d .
H6 H 0.4332 0.2722 1.0837 0.029 Uiso 1 1 calc R
N7 N 0.3237(2) 0.2277(2) 0.9005(4) 0.0170(8) Uani 1 1 d .
C8 C 0.2790(3) 0.1549(3) 0.8899(5) 0.0166(9) Uani 1 1 d .
C9 C 0.2029(3) 0.1298(3) 0.7519(5) 0.0244(11) Uani 1 1 d .
H9A H 0.2198 0.1126 0.6689 0.037 Uiso 1 1 calc R
H9B H 0.1637 0.1790 0.7173 0.037 Uiso 1 1 calc R
H9C H 0.1746 0.0812 0.7777 0.037 Uiso 1 1 calc R
C10 C 0.3072(3) 0.2961(3) 0.7844(6) 0.0222(11) Uani 1 1 d .
H10A H 0.3133 0.3530 0.8356 0.027 Uiso 1 1 calc R
H10B H 0.2478 0.2911 0.7066 0.027 Uiso 1 1 calc R
C11 C 0.3664(3) 0.2928(3) 0.7025(5) 0.0162(10) Uani 1 1 d .
C12 C 0.4134(3) 0.3649(3) 0.7009(5) 0.0165(10) Uani 1 1 d .
H12 H 0.4098 0.4157 0.7542 0.020 Uiso 1 1 calc R
C13 C 0.4656(3) 0.3637(3) 0.6220(5) 0.0154(9) Uani 1 1 d .
H13 H 0.4971 0.4139 0.6212 0.018 Uiso 1 1 calc R
C14 C 0.4727(3) 0.2905(3) 0.5444(5) 0.0140(9) Uani 1 1 d .
C15 C 0.4270(3) 0.2171(3) 0.5500(5) 0.0150(9) Uani 1 1 d .
H15 H 0.4323 0.1655 0.5001 0.018 Uiso 1 1 calc R
C16 C 0.3743(3) 0.2182(3) 0.6267(5) 0.0179(10) Uani 1 1 d .
H16 H 0.3432 0.1678 0.6281 0.021 Uiso 1 1 calc R
C17 C 0.4215(5) 0.0000 0.7891(10) 0.042(2) Uani 1 2 d S
H17A H 0.4587 0.0231 0.7429 0.062 Uiso 0.50 1 calc PR
H17B H 0.4387 -0.0592 0.8247 0.062 Uiso 0.50 1 calc PR
H17C H 0.4259 0.0361 0.8770 0.062 Uiso 0.50 1 calc PR
O18 O 0.3351(3) 0.0000 0.6756(6) 0.0399(14) Uani 1 2 d S
H18 H 0.3346 0.0000 0.5866 0.048 Uiso 1 2 calc SR
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'
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
N4 Co1 N4 115.6(2) . 6
N4 Co1 Cl2 110.03(11) . .
N4 Co1 Cl2 110.03(11) 6 .
N4 Co1 Cl3 103.15(11) . .
N4 Co1 Cl3 103.15(11) 6 .
Cl2 Co1 Cl3 114.74(8) . .
C8 N4 C5 105.9(4) . .
C8 N4 Co1 129.7(3) . .
C5 N4 Co1 124.2(3) . .
C6 C5 N4 109.6(4) . .
C6 C5 H5 125.2 . .
N4 C5 H5 125.2 . .
C5 C6 N7 106.3(4) . .
C5 C6 H6 126.8 . .
N7 C6 H6 126.8 . .
C8 N7 C6 108.0(4) . .
C8 N7 C10 128.2(4) . .
C6 N7 C10 123.8(4) . .
N4 C8 N7 110.2(4) . .
N4 C8 C9 125.6(4) . .
N7 C8 C9 124.1(4) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N7 C10 C11 113.3(4) . .
N7 C10 H10A 108.9 . .
C11 C10 H10A 108.9 . .
N7 C10 H10B 108.9 . .
C11 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C12 C11 C16 118.7(4) . .
C12 C11 C10 119.9(4) . .
C16 C11 C10 121.4(4) . .
C11 C12 C13 120.5(4) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C14 C13 C12 121.1(4) . .
C14 C13 H13 119.5 . .
C12 C13 H13 119.5 . .
C13 C14 C15 118.2(4) . .
C13 C14 C14 120.7(3) . 2_656
C15 C14 C14 121.0(3) . 2_656
C16 C15 C14 120.9(4) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C15 C16 C11 120.5(4) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
O18 C17 H17A 109.5 . .
O18 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O18 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C17 O18 H18 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl2 Co1 2.2701(19) .
Cl3 Co1 2.2811(19) .
Co1 N4 2.001(4) .
Co1 N4 2.001(4) 6
N4 C8 1.328(5) .
N4 C5 1.387(6) .
C5 C6 1.341(7) .
C5 H5 0.9500 .
C6 N7 1.376(6) .
C6 H6 0.9500 .
N7 C8 1.345(6) .
N7 C10 1.469(6) .
C8 C9 1.476(6) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.513(6) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.383(6) .
C11 C16 1.395(6) .
C12 C13 1.386(6) .
C12 H12 0.9500 .
C13 C14 1.382(6) .
C13 H13 0.9500 .
C14 C15 1.395(6) .
C14 C14 1.497(8) 2_656
C15 C16 1.375(6) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 O18 1.436(9) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O18 H18 0.8400 .
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
O18 H18 Cl3 0.84 2.36 3.203(6) 175.8 1_554
