Isolation of bridging and terminal coinage metal-nitrene complexes.
Dielmann, Fabian; Andrada, Diego M.; Frenking, Gernot; Bertrand, Guy; Journal of the American Chemical Society 136 (2014) 3800–3802; doi:10.1021/ja5007355

data_4129246
_publ_section_title
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 Isolation of bridging and terminal coinage metal-nitrene complexes.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3800
_journal_page_last               3802
_journal_paper_doi               10.1021/ja5007355
_journal_volume                  136
_journal_year                    2014
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C56 H76 Cu2 F6 N7 O6 P S2'
_chemical_formula_sum            'C56 H76 Cu2 F6 N7 O6 P S2'
_chemical_formula_weight         1279.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Jul 11 13:05:25 2013'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 107.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2148(12)
_cell_length_b                   15.3370(8)
_cell_length_c                   22.5133(11)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.63
_cell_measurement_theta_min      2.30
_cell_volume                     6665.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
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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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0405
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41188
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.78
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0485 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.9462.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.132
_platon_squeeze_details
;
The difference map peaklist indicates that one disordered pentane molecule per 
asymmetric unit sits on a special position. It was impossible to refine any 
reasonable molecule from difference Fourier peaks. Therefore the midpoint, the 
size and the number of electrons in that void were refined and the contribution 
to the calculated structure factors of the disordered solvent is taken into account
by back-Fourier transformation with the program SQUEEZE (Sluis and Spek, 1990). 
Two voids were found in the unit cell with 168 electrons in each void. This 
electron number corresponds to four pentane molecules in each void.
;
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+27.7662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                5616
_reflns_number_total             6820
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            ja5007355_si_001.cif
_cod_data_source_block           2a-DF457
_cod_database_code               4129246
_olex2_refinement_description
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1. Others
 Fixed Sof: F1A(0.75) F2A(0.75) F3A(0.75) O1A(0.75) O2A(0.75) O3A(0.75)
 C28A(0.75) F1B(0.25) F2B(0.25) F3B(0.25) O1B(0.25) O2B(0.25) O3B(0.25)
 C28B(0.25)
 Fixed U12: P1(0) N1(0)
 Fixed U23: P1(0) N1(0)
 Fixed Uiso: H2A(0.025) H2B(0.025) H3A(0.02) H3B(0.02) H6(0.023) H7(0.029)
 H8(0.023) H13(0.018) H14A(0.052) H14B(0.052) H14C(0.052) H15A(0.035)
 H15B(0.035) H15C(0.035) H18(0.026) H19(0.03) H20(0.025) H22(0.023) H23A(0.045)
 H23B(0.045) H23C(0.045) H24A(0.055) H24B(0.055) H24C(0.055) H25(0.022)
 H26A(0.044) H26B(0.044) H26C(0.044) H27A(0.054) H27B(0.054) H27C(0.054)
 H10(0.017) H11A(0.032) H11B(0.032) H11C(0.032) H12A(0.034) H12B(0.034)
 H12C(0.034)
 Fixed X: P1(1) N1(1) H2A(0.941) H2B(0.9252) H3A(1.0364) H3B(1.055) H6(0.756)
 H7(0.6973) H8(0.7525) H13(0.9248) H14A(0.7909) H14B(0.8605) H14C(0.8381)
 H15A(0.8983) H15B(0.8981) H15C(0.8279) H18(1.2755) H19(1.2884) H20(1.1986)
 H22(1.0281) H23A(1.0768) H23B(1.0004) H23C(1.0303) H24A(1.1) H24B(1.0455)
 H24C(1.1222) H25(1.1173) H26A(1.1616) H26B(1.1796) H26C(1.2365) H27A(1.2568)
 H27B(1.2003) H27C(1.1943) H10(0.9346) H11A(0.862) H11B(0.8877) H11C(0.8121)
 H12A(0.8269) H12B(0.9023) H12C(0.8892)
 Fixed Y: H2A(0.8372) H2B(0.7366) H3A(0.7167) H3B(0.8149) H6(0.9417)
 H7(0.8198) H8(0.6863) H13(0.64) H14A(0.5691) H14B(0.5218) H14C(0.6051)
 H15A(0.6301) H15B(0.5374) H15C(0.5846) H18(0.7541) H19(0.6053) H20(0.5162)
 H22(0.5884) H23A(0.4639) H23B(0.4698) H23C(0.5439) H24A(0.5218) H24B(0.4545)
 H24C(0.4513) H25(0.8705) H26A(0.861) H26B(0.9518) H26C(0.879) H27A(0.8893)
 H27B(0.9623) H27C(0.878) H10(0.9539) H11A(0.9483) H11B(1.0433) H11C(1.0156)
 H12A(1.057) H12B(1.09) H12C(1.0214)
 Fixed Z: P1(0.25) N1(0.25) H2A(0.0099) H2B(0.0121) H3A(0.019) H3B(0.0382)
 H6(0.0903) H7(0.1046) H8(0.1227) H13(0.1216) H14A(0.0666) H14B(0.0695)
 H14C(0.0281) H15A(0.2169) H15B(0.1875) H15C(0.1826) H18(0.2216) H19(0.2231)
 H20(0.1725) H22(0.0854) H23A(0.1813) H23B(0.1377) H23C(0.1862) H24A(0.0339)
 H24B(0.0433) H24C(0.0866) H25(0.1538) H26A(0.2631) H26B(0.2399) H26C(0.2589)
 H27A(0.1534) H27B(0.1335) H27C(0.0929) H10(0.097) H11A(-0.0082) H11B(0.0121)
 H11C(0.0089) H12A(0.1173) H12B(0.1245) H12C(0.1714)
;