Dinuclear cobalt(iii) and mixed valence trinuclear MnIII‒MnII‒MnIIIcomplexes with a tripodal bridging pyridylaminophenol ligand
Davila, Ruben; Farias, Nicolas; Carolina Sañudo, E.; Vega, Andrés; Escuer, Albert; Soler, Mónica; Manzur, Jorge; New J. Chem. 40 (2016) 6164–; doi:10.1039/C5NJ03670D

data_7055544
_publ_section_title
;
 Dinuclear cobalt(iii) and mixed valence trinuclear
 MnIII--MnII--MnIIIcomplexes with a tripodal bridging pyridylaminophenol
 ligand
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              6164
_journal_paper_doi               10.1039/C5NJ03670D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C50 H56 Mn3 N4 O10, (C4 H10 O)2'
_chemical_formula_sum            'C58 H76 Mn3 N4 O12'
_chemical_formula_weight         1186.06
_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     direct
_atom_sites_solution_secondary   difference
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-08 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                78.054(13)
_cell_angle_beta                 89.491(13)
_cell_angle_gamma                64.271(11)
_cell_formula_units_Z            2
_cell_length_a                   11.829(4)
_cell_length_b                   12.643(4)
_cell_length_c                   21.233(6)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.27
_cell_volume                     2786.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19768
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.835
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       plate
_exptl_crystal_F_000             1037.81
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
From thermogravimetry experiences, the 13.3% of weight loss at 55\%C is attributed
to two solvating ether molecules per trimer, which are incorporated into 
the reported formula
;
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_gt           0.1307
_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^)+(0.1995P)^2^+12.9173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3185
_refine_ls_wR_factor_ref         0.3482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7131
_reflns_number_total             10747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03670d2.cif
_cod_data_source_block           scd_68_1_p-1_new_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Triclinic' changed to
'triclinic' 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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055543--7055544.cif.
;
_cod_original_cell_volume        2787.1(15)
_cod_database_code               7055544
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              8170