Isolation of Neutral Mononuclear Copper Complexes Stabilized by Two Cyclic (Alkyl)(amino)carbenes.
Weinberger, David S.; Amin Sk, Nurul; Mondal, Kartik Chandra; Melaimi, Mohand; Bertrand, Guy; Stückl, A Claudia; Roesky, Herbert W.; Dittrich, Birger; Demeshko, Serhiy; Schwederski, Brigitte; Kaim, Wolfgang; Jerabek, Paul; Frenking, Gernot; Journal of the American Chemical Society 136 (2014) 6235–6238; doi:10.1021/ja502521b

data_4121697
_publ_section_title
;
 Isolation of Neutral Mononuclear Copper Complexes Stabilized by Two
 Cyclic (Alkyl)(amino)carbenes.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6235
_journal_page_last               6238
_journal_paper_doi               10.1021/ja502521b
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         '2(C22 H35 Cu0.5 N)'
_chemical_formula_sum            'C44 H70 Cu N2'
_chemical_formula_weight         690.56
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-03-01
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                86.172(2)
_cell_angle_beta                 84.756(2)
_cell_angle_gamma                76.646(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5174(3)
_cell_length_b                   12.0455(3)
_cell_length_c                   17.6337(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1956.49(10)
_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
;
XL, 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      296.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40843
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            '? reddish ?'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0376P)^2^+1.1240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                6949
_reflns_number_total             7958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja502521b_si_003.cif
_cod_data_source_block           gb_dsw024_0m
_cod_depositor_comments
'Adding full bibliography for 4121695--4121697.cif.'
_cod_database_code               4121697
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed X: Cu1(0.5) Cu2(0)
 Fixed Y: Cu1(0) Cu2(0.5)
 Fixed Z: Cu1(0.5) Cu2(1)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C39(H39), C42(H42)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C7(H7a,H7b), C25(H25a,H25b), C27(H27a,H27b),
 C29(H29a,H29b)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C35(H35), C36(H36), C37(H37)
3.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C26(H26a,H26b,H26c), C28(H28a,H28b,H28c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C40(H40a,H40b,H40c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c),
 C44(H44a,H44b,H44c)
;