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_7210395
_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            'C48 H56 Cl2 Cu5 N12 O18'
_chemical_formula_weight         1477.65
_chemical_name_common            '[Cu5]-tzp'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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                 100.018(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6809(3)
_cell_length_b                   10.7919(3)
_cell_length_c                   20.7122(5)
_cell_measurement_reflns_used    6236
_cell_measurement_temperature    149.8
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.9901
_cell_volume                     2791.27(12)
_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-97/2 (Sheldrick,1997)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      149.8
_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  -28.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  -96.0000  -59.0000 47
  
  2 omega  -85.00  -37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  179.0000  150.0000 48
  
  3 omega   16.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   77.0000 -180.0000 61
  
  4 omega    7.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -96.0000  119.0000 51
  
  5 omega   -3.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   37.0000   90.0000 98
  
  6 omega  -42.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -37.0000  -90.0000 91
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0100310000
_diffrn_orient_matrix_UB_12      0.0074661000
_diffrn_orient_matrix_UB_21      0.0298382000
_diffrn_orient_matrix_UB_22      -0.0559220000
_diffrn_orient_matrix_UB_23      0.0030401000
_diffrn_orient_matrix_UB_31      -0.0472843000
_diffrn_orient_matrix_UB_32      -0.0337119000
_diffrn_orient_matrix_UB_33      -0.0122175000
_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  0.0547
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23235
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81554
_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    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1502
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0362P)^2^+2.5861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                3963
_reflns_number_total             5090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40859k.txt
_cod_data_source_block           cmd216a3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7210395