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_4129247
_publ_section_title
;
 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_formula_moiety         'C56 H76 Ag2 F6 N7 O6 P S2, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H92 Ag2 F6 N7 O8 P S2'
_chemical_formula_weight         1512.28
_chemical_name_systematic        DF489
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                98.235(2)
_cell_angle_beta                 98.559(2)
_cell_angle_gamma                106.927(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4071(5)
_cell_length_b                   12.6841(5)
_cell_length_c                   23.8570(9)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.67
_cell_volume                     3482.0(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61314
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6814
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.133
_refine_diff_density_max         4.076
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         15966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0624P)^2^+12.6674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                13810
_reflns_number_total             15966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5007355_si_001.cif
_cod_data_source_block           2b-DF489
_cod_database_code               4129247
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.024) H2B(0.024) H3A(0.023) H3B(0.023) H5A(0.017) H5B(0.017)
 H6A(0.016) H6B(0.016) H9(0.029) H10(0.03) H11(0.027) H13(0.023) H14A(0.045)
 H14B(0.045) H14C(0.045) H15A(0.046) H15B(0.046) H15C(0.046) H16(0.023)
 H17A(0.04) H17B(0.04) H17C(0.04) H18A(0.041) H18B(0.041) H18C(0.041)
 H21(0.032) H22(0.039) H23(0.037) H25(0.031) H26A(0.075) H26B(0.075)
 H26C(0.075) H27A(0.056) H27B(0.056) H27C(0.056) H28(0.031) H29A(0.054)
 H29B(0.054) H29C(0.054) H30A(0.06) H30B(0.06) H30C(0.06) H33(0.026) H34(0.029)
 H35(0.028) H37(0.023) H38A(0.051) H38B(0.051) H38C(0.051) H39A(0.055)
 H39B(0.055) H39C(0.055) H40(0.022) H41A(0.035) H41B(0.035) H41C(0.035)
 H42A(0.036) H42B(0.036) H42C(0.036) H45(0.028) H46(0.035) H47(0.032)
 H49(0.017) H50A(0.028) H50B(0.028) H50C(0.028) H51A(0.03) H51B(0.03)
 H51C(0.03) H52(0.027) H53A(0.055) H53B(0.055) H53C(0.055) H54A(0.052)
 H54B(0.052) H54C(0.052) H57A(0.041) H57B(0.041) H58A(0.054) H58B(0.054)
 H59A(0.038) H59B(0.038) H60A(0.034) H60B(0.034) H61A(0.034) H61B(0.034)
 H62A(0.056) H62B(0.056) H63A(0.057) H63B(0.057) H64A(0.036) H64B(0.036)
 Fixed X: H2A(0.0333) H2B(-0.0502) H3A(0.0984) H3B(0.1813) H5A(-0.0703)
 H5B(0.0543) H6A(0.1318) H6B(0.0045) H9(-0.0738) H10(-0.2692) H11(-0.3466)
 H13(0.1388) H14A(0.0878) H14B(0.2083) H14C(0.1017) H15A(0.127) H15B(0.2254)
 H15C(0.1069) H16(-0.1922) H17A(-0.3028) H17B(-0.3701) H17C(-0.4019) H18A(-
 0.3374) H18B(-0.2562) H18C(-0.3746) H21(0.3617) H22(0.5218) H23(0.5221)
 H25(0.0872) H26A(0.1897) H26B(0.0585) H26C(0.1145) H27A(0.1927) H27B(0.1102)
 H27C(0.2417) H28(0.2827) H29A(0.3403) H29B(0.3995) H29C(0.4698) H30A(0.5184)
 H30B(0.4428) H30C(0.4174) H33(0.1256) H34(-0.0487) H35(-0.1908) H37(0.2052)
 H38A(0.2497) H38B(0.3137) H38C(0.1832) H39A(0.2789) H39B(0.3728) H39C(0.3042)
 H40(-0.1724) H41A(-0.3361) H41B(-0.2821) H41C(-0.3624) H42A(-0.2843) H42B(-
 0.1635) H42C(-0.2675) H45(0.0947) H46(0.2813) H47(0.3732) H49(-0.0901) H50A(-
 0.0976) H50B(-0.124) H50C(-0.2051) H51A(-0.1278) H51B(-0.0021) H51C(-0.0227)
 H52(0.2538) H53A(0.4252) H53B(0.4059) H53C(0.3134) H54A(0.3513) H54B(0.4333)
 H54C(0.4462) H57A(-0.4842) H57B(-0.4446) H58A(-0.5923) H58B(-0.5271) H59A(-
 0.4152) H59B(-0.4937) H60A(-0.2823) H60B(-0.3758) H61A(0.0804) H61B(0.191)
 H62A(0.2554) H62B(0.1812) H63A(0.3544) H63B(0.3868) H64A(0.3236) H64B(0.2427)
 Fixed Y: H2A(0.8255) H2B(0.7066) H3A(0.649) H3B(0.7636) H5A(1.0493)
 H5B(1.1368) H6A(0.9996) H6B(0.9196) H9(1.1457) H10(1.0596) H11(0.8666)
 H13(1.013) H14A(1.2082) H14B(1.1917) H14C(1.1162) H15A(1.0696) H15B(1.161)
 H15C(1.1801) H16(0.674) H17A(0.7113) H17B(0.5979) H17C(0.707) H18A(0.5745)
 H18B(0.6765) H18C(0.6811) H21(0.6134) H22(0.7704) H23(0.9201) H25(0.584)
 H26A(0.4853) H26B(0.4454) H26C(0.5619) H27A(0.5155) H27B(0.415) H27C(0.4594)
 H28(0.9501) H29A(1.0677) H29B(1.1329) H29C(1.0828) H30A(0.9824) H30B(1.0351)
 H30C(0.9046) H33(1.41) H34(1.3778) H35(1.2077) H37(1.2206) H38A(1.4545)
 H38B(1.4018) H38C(1.3881) H39A(1.2168) H39B(1.3) H39C(1.3468) H40(0.9731)
 H41A(1.0863) H41B(1.077) H41C(0.9688) H42A(0.8945) H42B(0.9663) H42C(1.0131)
 H45(0.5727) H46(0.6297) H47(0.8143) H49(0.7394) H50A(0.5123) H50B(0.5799)
 H50C(0.5539) H51A(0.6504) H51B(0.7347) H51C(0.6059) H52(1.0378) H53A(0.973)
 H53B(1.09) H53C(0.9809) H54A(1.0293) H54B(1.1169) H54C(0.9973) H57A(0.4724)
 H57B(0.5819) H58A(0.3924) H58B(0.4905) H59A(0.3939) H59B(0.2893) H60A(0.381)
 H60B(0.3271) H61A(0.6434) H61B(0.7016) H62A(0.5806) H62B(0.5869) H63A(0.7054)
 H63B(0.7498) H64A(0.8901) H64B(0.8143)
 Fixed Z: H2A(0.5145) H2B(0.5174) H3A(0.545) H3B(0.5361) H5A(0.9262)
 H5B(0.9501) H6A(0.9617) H6B(0.9552) H9(0.6043) H10(0.572) H11(0.5584)
 H13(0.6292) H14A(0.674) H14B(0.6898) H14C(0.7093) H15A(0.5399) H15B(0.5861)
 H15C(0.5679) H16(0.5804) H17A(0.6484) H17B(0.6049) H17C(0.5981) H18A(0.5014)
 H18B(0.482) H18C(0.4957) H21(0.7254) H22(0.7451) H23(0.7015) H25(0.6408)
 H26A(0.7226) H26B(0.6943) H26C(0.7368) H27A(0.5776) H27B(0.5975) H27C(0.6254)
 H28(0.6087) H29A(0.6993) H29B(0.6552) H29C(0.6982) H30A(0.6092) H30B(0.5706)
 H30C(0.5594) H33(0.819) H34(0.7601) H35(0.7458) H37(0.9015) H38A(0.9068)
 H38B(0.9512) H38C(0.9485) H39A(0.8172) H39B(0.8685) H39C(0.823) H40(0.8093)
 H41A(0.7879) H41B(0.85) H41C(0.806) H42A(0.718) H42B(0.7098) H42C(0.702)
 H45(0.8749) H46(0.8617) H47(0.8601) H49(0.8813) H50A(0.8547) H50B(0.8072)
 H50C(0.8514) H51A(0.9582) H51B(0.9763) H51C(0.9567) H52(0.873) H53A(0.8245)
 H53B(0.8255) H53C(0.7875) H54A(0.9628) H54B(0.9352) H54C(0.9341) H57A(0.6703)
 H57B(0.7189) H58A(0.7269) H58B(0.7804) H59A(0.8125) H59B(0.7646) H60A(0.759)
 H60B(0.7015) H61A(1.0698) H61B(1.1189) H62A(1.0658) H62B(1.0072) H63A(1.003)
 H63B(1.0707) H64A(1.0473) H64B(0.9893)
;