Synthesis and structural studies of metallamacrotricycles based on a metacyclophane in 1,3-alternate conformation bearing four imidazolyl units
Ehrhart, Jérôme; Planeix, Jean-Marc; Kyritsakas-Gruber, Nathalie; Hosseini, Mir Wais; Dalton Transactions  (2009) 2552–2557; doi:10.1039/b816053h

data_7000870
_publ_section_title
;
 Synthesis and structural studies of metallamacrotricycles based on a
 metacyclophane in 1,3-alternate conformation bearing four imidazolyl
 units
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2552
_journal_page_last               2557
_journal_paper_doi               10.1039/b816053h
_journal_year                    2009
_chemical_formula_moiety         'C56 H64 Br4 Hg2 N8, 5(C2 H2 Cl4)'
_chemical_formula_sum            'C66 H74 Br4 Cl20 Hg2 N8'
_chemical_formula_weight         2409.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   17.8054(16)
_cell_length_b                   18.6149(16)
_cell_length_c                   27.751(2)
_cell_measurement_reflns_used    5431
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.24
_cell_measurement_theta_min      2.16
_cell_volume                     9198.0(13)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            83112
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    5.694
_exptl_absorpt_correction_T_max  0.5028
_exptl_absorpt_correction_T_min  0.4272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.148
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         10575
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.579
_refine_ls_R_factor_all          0.2310
_refine_ls_R_factor_gt           0.1340
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1854P)^2^+243.5121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3065
_refine_ls_wR_factor_ref         0.3722
_reflns_number_gt                5106
_reflns_number_total             10575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816053h.txt
_cod_data_source_block           4-HgBr2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        9197.9(14)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7000870