A Series of [Co(Mabiq)Cl2-n] (n = 0, 1, 2) Compounds and Evidence for the Elusive Bimetallic Form.
Puttock, Emma V.; Banerjee, Priyabrata; Kaspar, Manuel; Drennen, Liam; Yufit, Dmitry S.; Bill, Eckhard; Sproules, Stephen; Hess, Corinna R.; Inorganic chemistry 54 (2015) 5864–5873; doi:10.1021/acs.inorgchem.5b00636

data_4343100
_publ_section_title
;
 A Series of [Co(Mabiq)Cl2-n] (n = 0, 1, 2) Compounds and Evidence for the
 Elusive Bimetallic Form.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5864
_journal_page_last               5873
_journal_paper_doi               10.1021/acs.inorgchem.5b00636
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C33 H33 Cl2 Co N8, C H2 Cl2'
_chemical_formula_sum            'C34 H35 Cl4 Co N8'
_chemical_formula_weight         756.43
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                101.466(2)
_cell_angle_beta                 104.309(2)
_cell_angle_gamma                103.074(2)
_cell_formula_units_Z            4
_cell_length_a                   10.0493(7)
_cell_length_b                   18.5861(13)
_cell_length_c                   19.4484(13)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.19
_cell_volume                     3301.4(4)
_computing_cell_refinement       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.30C (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, 
J.A.K. Howard, H. Puschmann, in preparation (2013)
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55117
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0846 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.9152.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         18354
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                13785
_reflns_number_total             18354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00636_si_002.cif
_cod_data_source_block           1_13srv251
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4343100--4343102.cif.
;
_cod_database_code               4343100
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4S-C2SA \\sim Cl3S-C2SA \\sim Cl3S-C2SB \\sim Cl3-C2SB
 with sigma of 0.005
3. Others
 Fixed Sof: Cl3(0.3) Cl4S(0.7) C2SA(0.7) H2SA(0.7) H2SB(0.7) C2SB(0.3)
 H2SC(0.3) H2SD(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2SA(H2SA,H2SB), C2SB(H2SC,H2SD)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C21(H21), C22(H22), C23(H23),
 C24(H24), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C14A(H14A), C21A(H21A),
 C22A(H22A), C23A(H23A), C24A(H24A)
4.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F), C32A(H32D,
 H32E,H32F), C33A(H33D,H33E,H33F)
;