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_7000869
_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         '4(C56 H64 Cl4 Cu2 N8), 9(C H Cl3), 10(H2 O)'
_chemical_formula_sum            'C233 H285 Cl43 Cu8 N32 O10'
_chemical_formula_weight         5726.60
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.011(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   16.9105(11)
_cell_length_b                   17.1432(13)
_cell_length_c                   25.9620(19)
_cell_measurement_reflns_used    1982
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.38
_cell_volume                     7525.2(9)
_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 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0875
_diffrn_reflns_av_sigmaI/netI    0.1702
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48792
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.9076
_exptl_absorpt_correction_T_min  0.8578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2950
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.935
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         15935
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.3804
_refine_ls_R_factor_gt           0.1534
_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^)+(0.2000P)^2^+0.8947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3893
_refine_ls_wR_factor_ref         0.4897
_reflns_number_gt                4085
_reflns_number_total             15935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816053h.txt
_cod_data_source_block           4-CuCl2
_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.

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)/n
_cod_database_code               7000869