Steric Control of a Bridging Ligand for High-Nuclearity Metallamacrocycle Formation: A Highly Puckered 60-Membered Icosanuclear Metalladiazamacrocycle
Moon, Dohyun; Lee, Kyungjae; John, Rohith P.; Kim, Ghyung Hwa; Suh, Byoung Jin; Lah, Myoung Soo; Inorganic Chemistry 45 (2006) 7991–7993; doi:10.1021/ic060646d

data_4332661
_publ_section_title
;
 Steric Control of a Bridging Ligand for High-Nuclearity Metallamacrocycle
 Formation:&#x00A0; A Highly Puckered 60-Membered Icosanuclear
 Metalladiazamacrocycle
;
_journal_issue                   20
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7991
_journal_page_last               7993
_journal_paper_doi               10.1021/ic060646d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C356 H328 Mn20 N40 O80 S18'
_chemical_formula_weight         8122.46
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   39.305(6)
_cell_length_b                   39.305(6)
_cell_length_c                   17.810(4)
_cell_measurement_reflns_used    23775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      1.32
_cell_volume                     27514(9)
_computing_cell_refinement       HKL2000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'DIAMOND 3.0'
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Silicon double crystal monochromator'
_diffrn_radiation_source         PAL
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.74999
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            87844
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   HKL2000-Scalepack
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8344
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         23775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1532P)^2^+19.3478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2239
_reflns_number_gt                20037
_reflns_number_total             23775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060646dsup1.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        27515(8)
_cod_original_sg_symbol_H-M      P4(2)/n
_cod_database_code               4332661