Progressive decoration of pentanuclear Cu(ii) 12-metallacrown-4 nodes towards targeted 1- and 2D extended networks
McDonald, Cecelia; Whyte, Teresa; Taylor, Stephanie M.; Sanz, Sergio; Brechin, Euan K.; Gaynor, Declan; Jones, Leigh F.; CrystEngComm 15 (2013) 6672–; doi:10.1039/c3ce40859k

data_7210393
_publ_section_title
;
 Progressive decoration of pentanuclear Cu(ii) 12-metallacrown-4 nodes
 towards targeted 1- and 2D extended networks
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6672
_journal_paper_doi               10.1039/c3ce40859k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C66 H70 Cl2 Cu5 N14 O16'
_chemical_formula_weight         1703.96
_chemical_name_common            '[Cu5(L)4(py)6](ClO4)2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.753(3)
_cell_angle_beta                 104.385(3)
_cell_angle_gamma                103.130(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3067(3)
_cell_length_b                   12.7372(5)
_cell_length_c                   13.2511(4)
_cell_measurement_reflns_used    8503
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.8764
_cell_volume                     1762.79(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -11.00   16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4216  -77.0000 -180.0000 27
  2 omega  -42.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8591  -77.0000   60.0000 95
  3 omega   -1.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8591   77.0000 -180.0000 93
  4 omega    6.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8591   77.0000  -30.0000 82
  5 omega   10.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.8591   37.0000  -30.0000 78
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0021765000
_diffrn_orient_matrix_UB_12      -0.0500633000
_diffrn_orient_matrix_UB_13      0.0182460000
_diffrn_orient_matrix_UB_21      -0.0672571000
_diffrn_orient_matrix_UB_22      -0.0142394000
_diffrn_orient_matrix_UB_23      -0.0169024000
_diffrn_orient_matrix_UB_31      -0.0000234000
_diffrn_orient_matrix_UB_32      -0.0264761000
_diffrn_orient_matrix_UB_33      -0.0506564000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13974
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.8764
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             871
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                5592
_reflns_number_total             6450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40859k.txt
_cod_data_source_block           cmd168a3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        1762.79(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210393