Anionic and zwitterionic copper(i) complexes incorporating an anionic N-heterocyclic carbene decorated with a malonate backbone: synthesis, structure and catalytic applications.
César, Vincent; Barthes, Cécile; Farré, Yoann C; Cuisiat, Stéphane V; Vacher, Bernard Y.; Brousses, Rémy; Lugan, Noël; Lavigne, Guy; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7373–7385; doi:10.1039/c3dt32919d

data_7021207
_publ_section_title
;
 Anionic and zwitterionic copper(i) complexes incorporating an anionic
 N-heterocyclic carbene decorated with a malonate backbone: synthesis,
 structure and catalytic applications.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7373
_journal_page_last               7385
_journal_paper_doi               10.1039/c3dt32919d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C111 H159 Cl3 Cu3 Li3 N6 O12'
_chemical_formula_sum            'C111 H159 Cl3 Cu3 Li3 N6 O12'
_chemical_formula_weight         2087.23
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3879(4)
_cell_length_b                   34.4666(13)
_cell_length_c                   31.0242(10)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      36.29
_cell_measurement_theta_min      2.09
_cell_measurement_wavelength     0.71073
_cell_volume                     14315.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            49831
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
After completing the initial structure solution, the cell
packing revealed a porous structure with channels running along the
a (x,0,0; x,1/2,0; x,1,0; x,0,1/2; x,1/2,1/2; x,1,1/2; x,0,1; x,1/2,1;
x,1,1) and c (1/2,0,z; 0,1/2,z; 1,1/2,z; 1/2,1,z) axis of approximately
5.4, and 3.5 angstroms in diameter, respectively. Residual Fourier maps
show these channels are likely to be filled with solvent(s), which, however,
could not be properly modelled in terms of discrete molecule sites. The SQUEEZE
procedure included in PLATON (PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998) procedure
was applied to the data.
;
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.695
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         14491
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.695
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1529P)^2^+1.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                11892
_reflns_number_total             14491
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt32919d.txt
_cod_data_source_block           2b_Li
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Orthorhombic' changed to
'orthorhombic' 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_database_code               7021207