Tetracarboxylate Ligands as New Chelates Supporting Copper(II) Paddlewheel-Like Structures.
Gomila, Antoine; Duval, Sylvain; Besnard, Céline; Krämer, Karl W; Liu, Shi-Xia; Decurtins, Silvio; Williams, Alan F.; Inorganic chemistry 53 (2014) 2683–2691; doi:10.1021/ic403077q

data_4337768
_publ_section_title
;
 Tetracarboxylate Ligands as New Chelates Supporting Copper(II)
 Paddlewheel-Like Structures.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2683
_journal_page_last               2691
_journal_paper_doi               10.1021/ic403077q
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C184 H184 Cu8 N16 O40, 3.2(C4 H10 O), 2.2(C3 H7 N1 O1)'
_chemical_formula_sum            'C203.4 H231.4 Cu8 N18.2 O45.4'
_chemical_formula_weight         4165.79
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-27
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   31.4137(6)
_cell_length_b                   31.4137(6)
_cell_length_c                   10.8904(3)
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      73.8901
_cell_measurement_theta_min      2.8110
_cell_volume                     10746.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
superflip
Palatinus L., Chapuis G. (2007.  J. Appl. Cryst. 40, 786-790,
;
_diffrn_ambient_temperature      190.15
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -46.00   34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3966   38.0000 -120.0000 80

  2 omega -115.00  -89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3966  -99.0000   30.0000 26

  3 omega   65.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3966 -125.0000 -120.0000 26

  4 omega   31.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -30.0000  -30.0000 27

  5 omega   31.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -30.0000  -60.0000 37

  6 omega  137.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  125.0000   30.0000 36

  7 omega   37.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -45.0000    0.0000 62

  8 omega   37.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.5399  -45.0000 -180.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0183339000
_diffrn_orient_matrix_UB_12      0.0454123000
_diffrn_orient_matrix_UB_13      -0.0081212000
_diffrn_orient_matrix_UB_21      0.0427053000
_diffrn_orient_matrix_UB_22      -0.0159867000
_diffrn_orient_matrix_UB_23      0.0521405000
_diffrn_orient_matrix_UB_31      0.0157360000
_diffrn_orient_matrix_UB_32      -0.0091164000
_diffrn_orient_matrix_UB_33      -0.1312860000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11334
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.05
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  1.811
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4349
_exptl_crystal_size_max          0.7468
_exptl_crystal_size_mid          0.0805
_exptl_crystal_size_min          0.0626
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
Space-group is non-centrosymmetric but contains symmetry elements of
the second kind.
Flack H D (1983), Acta Cryst. A39, 876-881
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         7956
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                7261
_reflns_number_total             7956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403077q_si_002.cif
_cod_data_source_block           cu8
_cod_original_formula_sum        'C203.40 H231.40 Cu8 N18.20 O45.40'
_cod_database_code               4337768
_chemical_oxdiff_formula         'Cu2 H58 C51 N4.55 O11.35'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97