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_7000866
_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
'2(C56 H64 Br4 CO2 N8), 3.60(C2 H4 Cl2), C H3 OH'
_chemical_formula_sum            'C120.2 H146.4 Br8 Cl7.2 Co4 N16 O'
_chemical_formula_weight         2951.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.952(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.0347(10)
_cell_length_b                   20.1741(9)
_cell_length_c                   15.5101(6)
_cell_measurement_reflns_used    6270
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.21
_cell_volume                     7051.4(5)
_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  0.1026
_diffrn_reflns_av_sigmaI/netI    0.1159
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70499
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    2.910
_exptl_absorpt_correction_T_max  0.7596
_exptl_absorpt_correction_T_min  0.5937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2986
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.836
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         16208
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1857P)^2^+73.1702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2860
_refine_ls_wR_factor_ref         0.3037
_reflns_number_gt                8650
_reflns_number_total             16208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816053h.txt
_cod_data_source_block           e1445a
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-12

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.

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_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C120.20 H146.40 Br8 Cl7.20 Co4 N16 O'
_cod_database_code               7000866