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_4337769
_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_formula_moiety         'C104 H100 Cu4 N8 O20, 4(C3 H7 N O)'
_chemical_formula_sum            'C116 H128 Cu4 N12 O24'
_chemical_formula_weight         2328.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2012-07-16
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2196(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.86902(13)
_cell_length_b                   18.90939(14)
_cell_length_c                   23.3517(2)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    179.9
_cell_measurement_theta_max      73.1767
_cell_measurement_theta_min      3.0141
_cell_volume                     5637.47(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      179.9
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -50.00   42.00   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865   38.0000  120.0000 115

  2 omega -113.00   -5.80   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865  -57.0000 -150.0000 134

  3 omega    9.00   34.60   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865   38.0000    0.0000 32

  4 omega   57.00  120.20   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       37.6865  178.0000  -90.0000 79

  5 omega  149.00  175.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000   30.0000 33

  6 omega   31.00  141.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -61.0000   30.0000 138

  7 omega   34.00   89.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -113.0000  -24.0000 69

  8 omega   32.00   76.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -180.0000 55

  9 omega   97.00  172.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000 -180.0000 94

 10 omega   55.00   99.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  120.0000 55

 11 omega   43.00   90.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -150.0000 59

 12 omega  146.00  172.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000  120.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0351102000
_diffrn_orient_matrix_UB_12      0.0019139000
_diffrn_orient_matrix_UB_13      -0.0607072000
_diffrn_orient_matrix_UB_21      -0.1004830000
_diffrn_orient_matrix_UB_22      -0.0396531000
_diffrn_orient_matrix_UB_23      -0.0243923000
_diffrn_orient_matrix_UB_31      -0.0568678000
_diffrn_orient_matrix_UB_32      0.0711049000
_diffrn_orient_matrix_UB_33      -0.0119824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20713
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         73.33
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.2707
_exptl_crystal_size_mid          0.0996
_exptl_crystal_size_min          0.0395
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10996
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0560P)^2^+1.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                9082
_reflns_number_total             10996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403077q_si_002.cif
_cod_data_source_block           cu4DMF
_cod_database_code               4337769
_chemical_oxdiff_formula         'Cu4 C116 N12 O24 H128'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97