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_4121695
_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         '3(I), 3(C44 H70 Cu N2), 10(C H Cl3)'
_chemical_formula_sum            'C142 H220 Cl30 Cu3 I3 N6'
_chemical_formula_weight         3646.05
_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
_audit_creation_date             2014-04-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                72.796(3)
_cell_angle_beta                 72.890(2)
_cell_angle_gamma                77.158(2)
_cell_formula_units_Z            1
_cell_length_a                   15.9571(12)
_cell_length_b                   16.2774(13)
_cell_length_c                   18.1897(14)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.36
_cell_volume                     4265.9(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f 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  0.0676
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49762
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.209
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0926 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.8231.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.120
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         17217
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+10.8631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11722
_reflns_number_total             17217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502521b_si_002.cif
_cod_data_source_block           gb_dsw_041_0m_a_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4121695--4121697.cif.
;
_cod_database_code               4121695
_shelxl_version_number           2013-4
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: Cl18(0.5) H67A(0.5) H67(0.5) Cl2(0.5)
4.a Ternary CH refined with riding coordinates:
 C42(H42), C57(H57), C13(H13), C20(H20), C35(H35), C64(H64), C69(H69),
 C68(H68), C71(H71), C70(H70), C67(H67A), C67(H67)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C49(H49A,H49B), C5(H5A,H5B), C7(H7A,H7B), C29(H29A,H29B),
 C47(H47A,H47B), C51(H51A,H51B), C25(H25A,H25B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C38(H38), C18(H18), C39(H39), C40(H40), C62(H62),
 C60(H60), C61(H61)
4.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C10(H10A,H10B,H10C), C53(H53A,H53B,
 H53C), C44(H44A,H44B,H44C), C9(H9A,H9B,H9C), C48(H48A,H48B,H48C), C59(H59A,
 H59B,H59C), C58(H58A,H58B,H58C), C15(H15A,H15B,H15C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C54(H54A,H54B,
 H54C), C22(H22A,H22B,H22C), C65(H65A,H65B,H65C), C4(H4A,H4B,H4C), C6(H6A,H6B,
 H6C), C21(H21A,H21B,H21C), C66(H66A,H66B,H66C), C28(H28A,H28B,H28C), C26(H26A,
 H26B,H26C), C31(H31A,H31B,H31C)
;