#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:36:47 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048097.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_7048097
loop_
_publ_author_name
'Srinivasan, Anandi'
'Wang, Xiaoping'
'Clérac, Rodolphe'
'Rouzières, Mathieu'
'Falvello, Larry R.'
'McGrady, John E.'
'Hillard, Elizabeth A.'
_publ_section_title
;
 Temperature dependence of the spin state and geometry in tricobalt
 paddlewheel complexes with halide axial ligands.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16798
_journal_page_last               16806
_journal_paper_doi               10.1039/c8dt03833c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C2 H4 Cl2'
_chemical_formula_sum            'C42 H36 Cl2 Co3 I2 N12'
_chemical_formula_weight         1210.32
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0708(7)
_cell_length_b                   11.5118(6)
_cell_length_c                   14.2242(8)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.28
_cell_volume                     2133.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46630
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.769
_exptl_absorpt_coefficient_mu    2.774
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       needle
_exptl_crystal_F_000             1186
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloroethane'
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4914
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²+4.1520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4218
_reflns_number_total             4914
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03833c2.cif
_cod_data_source_block           4-CLCH22-120K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048090--7048108.cif.
;
_cod_database_code               7048097
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.93278(18) 0.0739(2) 0.11803(17) 0.0151(5) Uani 1 1 d . . . . .
H1 H 1.002404 0.097820 0.118780 0.018 Uiso 1 1 calc R U . . .
C2 C 0.90979(19) -0.0400(2) 0.09676(18) 0.0188(5) Uani 1 1 d . . . . .
H2 H 0.961700 -0.092281 0.080315 0.023 Uiso 1 1 calc R U . . .
C3 C 0.8089(2) -0.0771(2) 0.09983(19) 0.0214(5) Uani 1 1 d . . . . .
H3 H 0.790969 -0.155827 0.086858 0.026 Uiso 1 1 calc R U . . .
C4 C 0.73535(18) 0.0018(2) 0.12194(18) 0.0171(5) Uani 1 1 d . . . . .
H4 H 0.666337 -0.022685 0.125391 0.021 Uiso 1 1 calc R U . . .
C5 C 0.76232(17) 0.11869(19) 0.13945(15) 0.0107(4) Uani 1 1 d . . . . .
C6 C 0.43483(17) 0.2807(2) 0.17726(17) 0.0142(5) Uani 1 1 d . . . . .
H6 H 0.396032 0.325605 0.217741 0.017 Uiso 1 1 calc R U . . .
C7 C 0.38654(19) 0.2402(2) 0.09458(18) 0.0198(5) Uani 1 1 d . . . . .
H7 H 0.316006 0.256010 0.078324 0.024 Uiso 1 1 calc R U . . .
C8 C 0.4439(2) 0.1752(2) 0.03518(18) 0.0217(5) Uani 1 1 d . . . . .
H8 H 0.412004 0.143778 -0.021569 0.026 Uiso 1 1 calc R U . . .
C9 C 0.54625(19) 0.1563(2) 0.05835(17) 0.0178(5) Uani 1 1 d . . . . .
H9 H 0.585831 0.113229 0.017331 0.021 Uiso 1 1 calc R U . . .
C10 C 0.59240(17) 0.20147(19) 0.14368(16) 0.0112(4) Uani 1 1 d . . . . .
C11 C 0.96645(17) 0.5617(2) 0.17507(16) 0.0138(5) Uani 1 1 d . . . . .
H11 H 0.994609 0.540112 0.118053 0.017 Uiso 1 1 calc R U . . .
C12 C 0.9807(2) 0.6740(2) 0.20678(18) 0.0184(5) Uani 1 1 d . . . . .
H12 H 1.019175 0.727685 0.173128 0.022 Uiso 1 1 calc R U . . .
C13 C 0.9380(2) 0.7072(2) 0.28863(18) 0.0203(5) Uani 1 1 d . . . . .
H13 H 0.947802 0.783802 0.312527 0.024 Uiso 1 1 calc R U . . .
C14 C 0.88115(19) 0.6281(2) 0.33499(17) 0.0166(5) Uani 1 1 d . . . . .
H14 H 0.850457 0.650266 0.390614 0.020 Uiso 1 1 calc R U . . .
C15 C 0.86863(16) 0.51420(19) 0.29969(15) 0.0103(4) Uani 1 1 d . . . . .
C16 C 0.83126(18) 0.3447(2) -0.02685(16) 0.0137(5) Uani 1 1 d . . . . .
H16 H 0.891970 0.301898 -0.035370 0.016 Uiso 1 1 calc R U . . .
C17 C 0.76959(19) 0.3762(2) -0.10549(17) 0.0177(5) Uani 1 1 d . . . . .
H17 H 0.787882 0.356223 -0.166742 0.021 Uiso 1 1 calc R U . . .
C18 C 0.68012(19) 0.4378(2) -0.09394(17) 0.0173(5) Uani 1 1 d . . . . .
H18 H 0.636612 0.461480 -0.147182 0.021 Uiso 1 1 calc R U . . .
C19 C 0.65556(18) 0.4639(2) -0.00415(16) 0.0150(5) Uani 1 1 d . . . . .
H19 H 0.594889 0.506530 0.004862 0.018 Uiso 1 1 calc R U . . .
C20 C 0.71983(17) 0.42773(19) 0.07442(16) 0.0103(4) Uani 1 1 d . . . . .
Co1 Co 0.89929(2) 0.31736(3) 0.17321(2) 0.00822(7) Uani 1 1 d . . . . .
Co2 Co 0.750000 0.31834(4) 0.250000 0.00851(9) Uani 1 2 d S T P . .
I1 I 1.08706(2) 0.31947(2) 0.07852(2) 0.01633(5) Uani 1 1 d . . . . .
N1 N 0.86187(14) 0.15411(16) 0.13797(13) 0.0102(4) Uani 1 1 d . . . . .
N2 N 0.53487(14) 0.26010(16) 0.20428(13) 0.0104(4) Uani 1 1 d . . . . .
N3 N 0.91453(14) 0.48061(16) 0.22075(13) 0.0098(4) Uani 1 1 d . . . . .
N4 N 0.80987(14) 0.37154(16) 0.06212(13) 0.0102(4) Uani 1 1 d . . . . .
N5 N 0.69536(14) 0.20067(16) 0.16776(13) 0.0103(4) Uani 1 1 d . . . . .
N6 N 0.69499(14) 0.43363(16) 0.16593(13) 0.0104(4) Uani 1 1 d . . . . .
Cl1 Cl 0.1679(8) -0.0903(9) 0.3292(6) 0.083(4) Uani 0.232(2) 1 d D U P A -1
C21 C 0.2591(12) 0.0018(14) 0.3317(10) 0.052(3) Uani 0.232(2) 1 d D U P A -1
H21A H 0.237186 0.072527 0.364192 0.062 Uiso 0.232(2) 1 calc R U P A -1
H21B H 0.318676 -0.030928 0.370171 0.062 Uiso 0.232(2) 1 calc R U P A -1
C22 C 0.2934(13) 0.0364(11) 0.2395(12) 0.042(3) Uani 0.232(2) 1 d D U P A -1
H22A H 0.334177 0.108802 0.247026 0.050 Uiso 0.232(2) 1 calc R U P A -1
H22B H 0.232742 0.052476 0.195237 0.050 Uiso 0.232(2) 1 calc R U P A -1
Cl2 Cl 0.3690(6) -0.0737(9) 0.1916(7) 0.068(3) Uani 0.232(2) 1 d D U P A -1
Cl3 Cl 0.2856(9) -0.0790(12) 0.3662(9) 0.075(5) Uani 0.268(2) 1 d D U P A -2
C23 C 0.2891(15) 0.0384(11) 0.2840(11) 0.026(4) Uiso 0.268(2) 1 d D U P A -2
H23A H 0.294084 0.113253 0.318266 0.031 Uiso 0.268(2) 1 calc R U P A -2
H23B H 0.350026 0.030623 0.247364 0.031 Uiso 0.268(2) 1 calc R U P A -2
C24 C 0.1950(16) 0.0363(12) 0.2197(12) 0.030(4) Uiso 0.268(2) 1 d D U P A -2
H24A H 0.188099 0.110743 0.184864 0.036 Uiso 0.268(2) 1 calc R U P A -2
H24B H 0.134453 0.027405 0.256665 0.036 Uiso 0.268(2) 1 calc R U P A -2
Cl4 Cl 0.1992(6) -0.0814(7) 0.1376(7) 0.0269(13) Uani 0.268(2) 1 d D . P A -2
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'
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'
I I -0.4742 1.8119 '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'
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 C1 C2 123.8(2) . .
N1 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C1 C2 C3 118.6(2) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
C4 C3 C2 119.0(2) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 120.1(2) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
N1 C5 N5 115.53(19) . .
N1 C5 C4 120.5(2) . .
N5 C5 C4 123.6(2) . .
N2 C6 C7 123.5(2) . .
N2 C6 H6 118.3 . .
C7 C6 H6 118.3 . .
C6 C7 C8 118.0(2) . .
C6 C7 H7 121.0 . .
C8 C7 H7 121.0 . .
C9 C8 C7 120.2(2) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C9 C10 119.4(2) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N5 C10 N2 115.29(19) . .
N5 C10 C9 124.0(2) . .
N2 C10 C9 120.4(2) . .
N3 C11 C12 123.5(2) . .
N3 C11 H11 118.3 . .
C12 C11 H11 118.3 . .
C11 C12 C13 118.8(2) . .
C11 C12 H12 120.6 . .
C13 C12 H12 120.6 . .
C14 C13 C12 119.3(2) . .
C14 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
C13 C14 C15 119.8(2) . .
C13 C14 H14 120.1 . .
C15 C14 H14 120.1 . .
N6 C15 N3 114.94(19) 2_655 .
N6 C15 C14 124.2(2) 2_655 .
N3 C15 C14 120.6(2) . .
N4 C16 C17 123.3(2) . .
N4 C16 H16 118.3 . .
C17 C16 H16 118.3 . .
C16 C17 C18 118.9(2) . .
C16 C17 H17 120.5 . .
C18 C17 H17 120.5 . .
C19 C18 C17 118.9(2) . .
C19 C18 H18 120.6 . .
C17 C18 H18 120.6 . .
C18 C19 C20 120.3(2) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
N4 C20 N6 114.68(19) . .
N4 C20 C19 120.3(2) . .
N6 C20 C19 124.7(2) . .
N4 Co1 N2 169.59(8) . 2_655
N4 Co1 N1 88.80(8) . .
N2 Co1 N1 89.33(8) 2_655 .
N4 Co1 N3 90.59(7) . .
N2 Co1 N3 89.47(7) 2_655 .
N1 Co1 N3 169.95(8) . .
N4 Co1 Co2 84.79(5) . .
N2 Co1 Co2 84.86(5) 2_655 .
N1 Co1 Co2 85.64(6) . .
N3 Co1 Co2 84.31(5) . .
N4 Co1 I1 95.39(5) . .
N2 Co1 I1 94.98(5) 2_655 .
N1 Co1 I1 95.22(5) . .
N3 Co1 I1 94.83(5) . .
Co2 Co1 I1 179.118(16) . .
N6 Co2 N6 90.77(11) . 2_655
N6 Co2 N5 90.34(8) . .
N6 Co2 N5 178.85(8) 2_655 .
N6 Co2 N5 178.85(8) . 2_655
N6 Co2 N5 90.33(8) 2_655 2_655
N5 Co2 N5 88.56(11) . 2_655
N6 Co2 Co1 90.55(6) . 2_655
N6 Co2 Co1 89.84(6) 2_655 2_655
N5 Co2 Co1 89.85(6) . 2_655
N5 Co2 Co1 89.75(6) 2_655 2_655
N6 Co2 Co1 89.84(6) . .
N6 Co2 Co1 90.55(6) 2_655 .
N5 Co2 Co1 89.75(6) . .
N5 Co2 Co1 89.85(6) 2_655 .
Co1 Co2 Co1 179.44(2) 2_655 .
C1 N1 C5 117.95(19) . .
C1 N1 Co1 122.44(16) . .
C5 N1 Co1 119.48(15) . .
C6 N2 C10 118.36(19) . .
C6 N2 Co1 122.00(16) . 2_655
C10 N2 Co1 119.60(15) . 2_655
C11 N3 C15 117.96(19) . .
C11 N3 Co1 121.77(15) . .
C15 N3 Co1 120.23(15) . .
C16 N4 C20 118.17(19) . .
C16 N4 Co1 121.27(15) . .
C20 N4 Co1 120.28(15) . .
C10 N5 C5 124.93(19) . .
C10 N5 Co2 117.85(15) . .
C5 N5 Co2 117.18(15) . .
C15 N6 C20 124.99(19) 2_655 .
C15 N6 Co2 117.60(15) 2_655 .
C20 N6 Co2 117.39(15) . .
C22 C21 Cl1 116.1(11) . .
C22 C21 H21A 108.3 . .
Cl1 C21 H21A 108.2 . .
C22 C21 H21B 108.2 . .
Cl1 C21 H21B 108.2 . .
H21A C21 H21B 107.4 . .
C21 C22 Cl2 111.5(10) . .
C21 C22 H22A 109.3 . .
Cl2 C22 H22A 109.3 . .
C21 C22 H22B 109.3 . .
Cl2 C22 H22B 109.3 . .
H22A C22 H22B 108.0 . .
C24 C23 Cl3 109.3(10) . .
C24 C23 H23A 109.8 . .
Cl3 C23 H23A 109.8 . .
C24 C23 H23B 109.8 . .
Cl3 C23 H23B 109.8 . .
H23A C23 H23B 108.3 . .
C23 C24 Cl4 110.4(10) . .
C23 C24 H24A 109.6 . .
Cl4 C24 H24A 109.6 . .
C23 C24 H24B 109.6 . .
Cl4 C24 H24B 109.6 . .
H24A C24 H24B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.354(3) .
C1 C2 1.374(3) .
C1 H1 0.9500 .
C2 C3 1.390(4) .
C2 H2 0.9500 .
C3 C4 1.377(3) .
C3 H3 0.9500 .
C4 C5 1.408(3) .
C4 H4 0.9500 .
C5 N1 1.365(3) .
C5 N5 1.369(3) .
C6 N2 1.354(3) .
C6 C7 1.371(3) .
C6 H6 0.9500 .
C7 C8 1.392(4) .
C7 H7 0.9500 .
C8 C9 1.369(3) .
C8 H8 0.9500 .
C9 C10 1.411(3) .
C9 H9 0.9500 .
C10 N5 1.362(3) .
C10 N2 1.366(3) .
C11 N3 1.351(3) .
C11 C12 1.377(3) .
C11 H11 0.9500 .
C12 C13 1.385(4) .
C12 H12 0.9500 .
C13 C14 1.376(3) .
C13 H13 0.9500 .
C14 C15 1.409(3) .
C14 H14 0.9500 .
C15 N6 1.362(3) 2_655
C15 N3 1.370(3) .
C16 N4 1.353(3) .
C16 C17 1.374(3) .
C16 H16 0.9500 .
C17 C18 1.388(3) .
C17 H17 0.9500 .
C18 C19 1.375(3) .
C18 H18 0.9500 .
C19 C20 1.406(3) .
C19 H19 0.9500 .
C20 N4 1.366(3) .
C20 N6 1.368(3) .
Co1 N4 1.9892(18) .
Co1 N2 1.9931(19) 2_655
Co1 N1 1.9958(19) .
Co1 N3 2.0017(19) .
Co1 Co2 2.3111(3) .
Co1 I1 2.8925(4) .
Co2 N6 1.8898(19) .
Co2 N6 1.8898(19) 2_655
Co2 N5 1.8921(19) .
Co2 N5 1.8921(19) 2_655
Cl1 C21 1.594(15) .
C21 C22 1.474(14) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 Cl2 1.776(13) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
Cl3 C23 1.790(11) .
C23 C24 1.473(12) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 Cl4 1.792(11) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
