Modulation of the Ring Size and Nuclearity of Metallamacrocycles via the Steric Effect of Ligands: Preparation and Characterization of 18-Membered Hexanuclear, 24-Membered Octanuclear, and 30-Membered Decanuclear Manganese Metalladiazamacrocycles with α- and β-Branched N-Acylsalicylhydrazides
Rohith P. John; Kyungjae Lee; Beom Jin Kim; Byoung Jin Suh; Hackjune Rhee; Myoung Soo Lah; Inorganic Chemistry 44 (2005) 7109–7121; doi:10.1021/ic050891h

data_4309690
_publ_section_title
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Modulation of the Ring Size and Nuclearity of Metallamacrocycles via the
Steric Effect of Ligands: Preparation and Characterization of 18-Membered
Hexanuclear, 24-Membered Octanuclear, and 30-Membered Decanuclear Manganese
Metalladiazamacrocycles with \a- and \b-Branched N-Acylsalicylhydrazides
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7109
_journal_page_last               7121
_journal_paper_doi               10.1021/ic050891h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C168 H246 Mn10 N36 O48'
_chemical_formula_weight         4087.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 118.755(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   39.187(5)
_cell_length_b                   20.494(5)
_cell_length_c                   28.283(5)
_cell_measurement_reflns_used    5731
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.22
_cell_volume                     19913(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1490
_diffrn_reflns_av_sigmaI/netI    0.2432
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61214
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.8188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         23634
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.3130
_refine_ls_R_factor_gt           0.1044
_refine_ls_shift/su_max          4.111
_refine_ls_shift/su_mean         0.119
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2527
_refine_ls_wR_factor_ref         0.3435
_reflns_number_gt                6006
_reflns_number_total             23634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050891hc1_7.cif
_cod_data_source_block           complex5b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4309690