Enhancing the ferromagnetic coupling in extended phloroglucinol complexes by increasing the metal SOMO-ligand overlap: synthesis and characterization of a trinuclear Co triplesalophen complex.
Oldengott, Jan; Stammler, Anja; Bögge, Hartmut; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9732–9735; doi:10.1039/c5dt01255d

data_7034821
_publ_section_title
;
 Enhancing the ferromagnetic coupling in extended phloroglucinol complexes
 by increasing the metal SOMO-ligand overlap: synthesis and
 characterization of a trinuclear Co triplesalophen complex.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9732
_journal_page_last               9735
_journal_paper_doi               10.1039/c5dt01255d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C69 H48 Co3 N6 O6, H2 O , C2 H4 Cl2'
_chemical_formula_sum            'C71 H54 Cl2 Co3 N6 O7'
_chemical_formula_weight         1350.89
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-17 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                73.5170(10)
_cell_angle_beta                 89.290(2)
_cell_angle_gamma                74.132(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2547(3)
_cell_length_b                   16.1141(5)
_cell_length_c                   18.9659(5)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.63
_cell_measurement_theta_min      4.37
_cell_volume                     2883.48(15)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 v2012.12-0 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR ULTRA'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM Montel Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_laue_measured_fraction_full 0.975
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57571
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        66.499
_diffrn_reflns_theta_max         66.499
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'I\mS Incoatec Microfocus Source'
_diffrn_source_type              'Bruker X8 PROSPECTOR ULTRA'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.064
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0900 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.6194.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       column
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
One C2H4Cl2 molecule was originally found in the asymmetric unit, which,
however, suffered from strong disorder and could not be refined properly. 
Thus, it was removed from the coordinate set and its scattering power determined
using the PLATON/SQUEEZE routine, which finds approx. 40 e- per complex molecule
in the solvent region. This corresponds to approx. 1 C2H4Cl2 molecule per
complex molecule, which is therefore included in the given sum formula 
and derived quantities.
The structure factor contribution from this (.fab file) is added to that of the 
structure model. 

;
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         9930
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+2.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8768
_reflns_number_total             9930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01255d2.cif
_cod_data_source_block           g2359f_sq_s
_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/RSC/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 7034821.cif.
;
_cod_database_code               7034821
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C395) \\sim Ueq, Uanis(C394) \\sim Ueq, Uanis(C393) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C24(H24),
 C25(H25), C26(H26), C27(H27), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37),
  C103(H103), C105(H105), C106(H106), C192(H192), C193(H193), C194(H194),
 C195(H195), C196(H196), C203(H203), C205(H205), C206(H206), C292(H292),
 C293(H293), C294(H294), C295(H295), C296(H296), C303(H303), C305(H305),
 C306(H306), C392(H392), C393(H393), C394(H394), C395(H395), C396(H396)
3.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C210(H21A,H21B,H21C), C310(H31A,H31B,H31C)
;
_shelx_res_checksum              55254
_shelx_fab_checksum              88018
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'