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_7210397
_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            'C32 H40 Cl2 Cu5 N8 O21'
_chemical_formula_weight         1261.32
_chemical_name_common            '[Cu5]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                110.321(3)
_cell_angle_beta                 96.075(3)
_cell_angle_gamma                96.316(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0640(3)
_cell_length_b                   12.2750(4)
_cell_length_c                   17.2399(6)
_cell_measurement_reflns_used    8283
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.8605
_cell_volume                     2156.10(13)
_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, McArdle, P. (1995) J.Appl.Cryst.,28,65-65
;
_computing_publication_material
;
 Ciftab, G.M. Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_computing_structure_refinement
;
 SHELXL-97/2, G.M. Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_computing_structure_solution
;
 SHELXS-97, Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_diffrn_ambient_temperature      150.0
_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  -17.00   58.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653   37.0000   30.0000 75
  
  2 omega  -58.00  -32.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  179.0000  150.0000 26
  
  3 omega   -1.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   77.0000  -90.0000 92
  
  4 omega  -41.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -77.0000  150.0000 94
  
  5 omega    1.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   83.0000    4.0000 32
  
  6 omega   13.00   84.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   77.0000   60.0000 71
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0348869000
_diffrn_orient_matrix_UB_12      -0.0429343000
_diffrn_orient_matrix_UB_21      -0.0510412000
_diffrn_orient_matrix_UB_22      -0.0269626000
_diffrn_orient_matrix_UB_23      -0.0323203000
_diffrn_orient_matrix_UB_31      0.0209707000
_diffrn_orient_matrix_UB_32      0.0363739000
_diffrn_orient_matrix_UB_33      -0.0216147000
_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  0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17735
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    2.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95013
_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    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.092
_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     614
_refine_ls_number_reflns         7876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0319P)^2^+2.2190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                6482
_reflns_number_total             7876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40859k.txt
_cod_data_source_block           tw19a2
_cod_original_cell_volume        2156.10(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210397