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_4309689
_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            'C165 H235 Mn10 N35 O45'
_chemical_formula_weight         3978.28
_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                90.00
_cell_angle_beta                 118.231(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.044(3)
_cell_length_b                   20.7050(17)
_cell_length_c                   28.139(2)
_cell_measurement_reflns_used    3665
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.22
_cell_volume                     20042(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1375
_diffrn_reflns_av_sigmaI/netI    0.1947
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43805
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.9345
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8320
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         14408
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.2326
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          7.717
_refine_ls_shift/su_mean         0.197
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.2583
_reflns_number_gt                4612
_reflns_number_total             14408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050891hc1_6.cif
_cod_data_source_block           complex5a
_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               4309689