Isolation of a potassium bis(1,2,3-triazol-5-ylidene)carbazolide: a stabilizing pincer ligand for reactive late transition metal complexes.
Bezuidenhout, Daniela I.; Kleinhans, George; Guisado-Barrios, Gregorio; Liles, David C.; Ung, Gaël; Bertrand, Guy; Chemical communications (Cambridge, England) 50 (2014) 2431–2433; doi:10.1039/c3cc49385g

data_7125614
_publ_section_title
;
 Isolation of a potassium bis(1,2,3-triazol-5-ylidene)carbazolide: a
 stabilizing pincer ligand for reactive late transition metal complexes.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2431
_journal_page_last               2433
_journal_paper_doi               10.1039/c3cc49385g
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C72 H90 K N7'
_chemical_formula_sum            'C72 H90 K N7'
_chemical_formula_weight         1092.60
_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
_audit_creation_date             2013-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                82.8410(11)
_cell_angle_beta                 74.7310(10)
_cell_angle_gamma                68.2340(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4327(3)
_cell_length_b                   14.6585(3)
_cell_length_c                   17.8114(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3374.50(13)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80987
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         2.573
_exptl_absorpt_coefficient_mu    1.016
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.064
_platon_squeeze_details
;
;
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         12717
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+1.1881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10297
_reflns_number_total             12717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49385g.txt
_cod_data_source_block           cu_gkle0087_0m_a
_cod_database_code               7125614
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Others
 Fixed Sof: C11A(0.25) H11A(0.25) H11B(0.25) H11C(0.25) C10(0.75) H10A(0.75)
 H10B(0.75) H10C(0.75) C12A(0.25) H12A(0.25) H12B(0.25) H12C(0.25) C10A(0.25)
 H10D(0.25) H10E(0.25) H10F(0.25) C11(0.75) H11D(0.75) H11E(0.75) H11F(0.75)
 C12(0.75) H12D(0.75) H12E(0.75) H12F(0.75)
 Fixed Uiso: H42(0.034) H44(0.034) H6(0.036) H8(0.035) H46A(0.096) H46B(0.096)
 H46C(0.096) H48A(0.099) H48B(0.099) H48C(0.099) H47A(0.155) H47B(0.155)
 H47C(0.155) H11A(0.069) H11B(0.069) H11C(0.069) H10A(0.133) H10B(0.133)
 H10C(0.133) H12A(0.089) H12B(0.089) H12C(0.089) H65(0.047) H64(0.051)
 H63(0.044) H67(0.042) H68A(0.073) H68B(0.073) H68C(0.073) H69A(0.096)
 H69B(0.096) H69C(0.096) H1(0.038) H71A(0.071) H71B(0.071) H71C(0.071)
 H72A(0.094) H72B(0.094) H72C(0.094) H51(0.053) H52(0.052) H53(0.046)
 H58(0.063) H59A(0.175) H59B(0.175) H59C(0.175) H60A(0.138) H60B(0.138)
 H60C(0.138) H55(0.039) H57A(0.085) H57B(0.085) H57C(0.085) H56A(0.083)
 H56B(0.083) H56C(0.083) H29(0.047) H28(0.054) H27(0.048) H31(0.04) H33A(0.084)
 H33B(0.084) H33C(0.084) H32A(0.089) H32B(0.089) H32C(0.089) H34(0.039)
 H36A(0.068) H36B(0.068) H36C(0.068) H35A(0.077) H35B(0.077) H35C(0.077)
 H17(0.044) H16(0.053) H15(0.051) H19(0.038) H20A(0.065) H20B(0.065)
 H20C(0.065) H21A(0.062) H21B(0.062) H21C(0.062) H22(0.05) H24A(0.093)
 H24B(0.093) H24C(0.093) H23A(0.116) H23B(0.116) H23C(0.116) H10D(0.078)
 H10E(0.078) H10F(0.078) H11D(0.121) H11E(0.121) H11F(0.121) H12D(0.15)
 H12E(0.15) H12F(0.15)
 Fixed X: H42(0.6961) H44(0.6651) H6(0.7486) H8(0.806) H46A(0.5082)
 H46B(0.4973) H46C(0.5083) H48A(0.7683) H48B(0.6646) H48C(0.6803) H47A(0.6609)
 H47B(0.6409) H47C(0.7518) H11A(0.7515) H11B(0.6862) H11C(0.8019) H10A(0.8443)
 H10B(0.7221) H10C(0.793) H12A(0.943) H12B(0.9002) H12C(0.8887) H65(0.4617)
 H64(0.458) H63(0.541) H67(0.5808) H68A(0.4047) H68B(0.4397) H68C(0.4004)
 H69A(0.6803) H69B(0.6119) H69C(0.5785) H1(0.6702) H71A(0.5409) H71B(0.6498)
 H71C(0.6093) H72A(0.7652) H72B(0.8095) H72C(0.8039) H51(0.9542) H52(1.0857)
 H53(1.0781) H58(0.7315) H59A(0.677) H59B(0.6586) H59C(0.7537) H60A(0.8536)
 H60B(0.7628) H60C(0.8682) H55(0.8651) H57A(0.9698) H57B(1.0028) H57C(1.071)
 H56A(1.0489) H56B(0.9646) H56C(0.9376) H29(0.6938) H28(0.8173) H27(0.9532)
 H31(0.6953) H33A(0.5694) H33B(0.518) H33C(0.5442) H32A(0.6409) H32B(0.622)
 H32C(0.7365) H34(0.9758) H36A(1.0643) H36B(1.0898) H36C(0.9788) H35A(1.0677)
 H35B(1.1462) H35C(1.1095) H17(0.9521) H16(1.0966) H15(1.1451) H19(0.7776)
 H20A(0.7873) H20B(0.6876) H20C(0.7332) H21A(0.8852) H21B(0.789) H21C(0.8968)
 H22(1.0131) H24A(1.0026) H24B(1.0927) H24C(1.1199) H23A(1.2207) H23B(1.1866)
 H23C(1.1623) H10D(0.714) H10E(0.6311) H10F(0.703) H11D(0.7343) H11E(0.6471)
 H11F(0.722) H12D(0.9155) H12E(0.9067) H12F(0.955)
 Fixed Y: H42(0.0115) H44(0.1495) H6(0.0491) H8(0.27) H46A(0.0201) H46B(0.079)
 H46C(-0.0343) H48A(-0.1274) H48B(-0.1074) H48C(-0.1637) H47A(-0.0821)
 H47B(0.033) H47C(-0.042) H11A(-0.0086) H11B(0.0356) H11C(-0.0395) H10A(0.182)
 H10B(0.2129) H10C(0.1183) H12A(0.0329) H12B(0.1392) H12C(0.0466) H65(0.6762)
 H64(0.806) H63(0.7766) H67(0.4199) H68A(0.5524) H68B(0.4351) H68C(0.4925)
 H69A(0.4729) H69B(0.4226) H69C(0.5397) H1(0.5429) H71A(0.6832) H71B(0.6614)
 H71C(0.7478) H72A(0.6759) H72B(0.596) H72C(0.5612) H51(0.0822) H52(0.0169)
 H53(0.0873) H58(0.2968) H59A(0.1676) H59B(0.1929) H59C(0.0992) H60A(0.1672)
 H60B(0.2698) H60C(0.2681) H55(0.2837) H57A(0.3613) H57B(0.3362) H57C(0.2697)
 H56A(0.1289) H56B(0.1992) H56C(0.1205) H29(0.848) H28(0.8571) H27(0.7163)
 H31(0.6274) H33A(0.6708) H33B(0.7177) H33C(0.7852) H32A(0.8331) H32B(0.7552)
 H32C(0.75) H34(0.4699) H36A(0.5822) H36B(0.4663) H36C(0.5412) H35A(0.5055)
 H35B(0.4547) H35C(0.571) H17(0.3426) H16(0.2049) H15(0.1491) H19(0.4803)
 H20A(0.4405) H20B(0.5079) H20C(0.392) H21A(0.569) H21B(0.6114) H21C(0.5392)
 H22(0.2635) H24A(0.1118) H24B(0.0948) H24C(0.0725) H23A(0.1889) H23B(0.2108)
 H23C(0.2995) H10D(0.2392) H10E(0.1924) H10F(0.1485) H11D(0.0001) H11E(0.0894)
 H11F(0.0009) H12D(-0.0263) H12E(-0.0308) H12F(0.043)
 Fixed Z: H42(0.4367) H44(0.6296) H6(0.2743) H8(0.1347) H46A(0.5626)
 H46B(0.6362) H46C(0.6463) H48A(0.5354) H48B(0.5088) H48C(0.5901) H47A(0.701)
 H47B(0.6995) H47C(0.6598) H11A(0.0903) H11B(0.1736) H11C(0.1639) H10A(0.0371)
 H10B(0.0577) H10C(0.0068) H12A(0.0908) H12B(0.0508) H12C(0.0205) H65(0.8002)
 H64(0.711) H63(0.581) H67(0.7564) H68A(0.8552) H68B(0.8623) H68C(0.7877)
 H69A(0.8143) H69B(0.8784) H69C(0.8719) H1(0.4955) H71A(0.4577) H71B(0.397)
 H71C(0.4574) H72A(0.5124) H72B(0.4462) H72C(0.5356) H51(0.755) H52(0.6484)
 H53(0.5251) H58(0.7562) H59A(0.7527) H59B(0.8415) H59C(0.8043) H60A(0.8553)
 H60B(0.879) H60C(0.8197) H55(0.4746) H57A(0.4958) H57B(0.4056) H57C(0.4636)
 H56A(0.408) H56B(0.3631) H56C(0.4273) H29(0.2516) H28(0.3083) H27(0.3275)
 H31(0.1804) H33A(0.2958) H33B(0.224) H33C(0.2733) H32A(0.142) H32B(0.0979)
 H32C(0.0918) H34(0.3048) H36A(0.3649) H36B(0.3778) H36C(0.4174) H35A(0.1819)
 H35B(0.2365) H35C(0.2202) H17(-0.0821) H16(-0.0778) H15(0.0383) H19(0.0844)
 H20A(-0.071) H20B(-0.012) H20C(0.0049) H21A(0.0311) H21B(-0.008) H21C(-0.0552)
 H22(0.2245) H24A(0.2092) H24B(0.2518) H24C(0.1613) H23A(0.1365) H23B(0.2274)
 H23C(0.1648) H10D(0.0594) H10E(0.1075) H10F(0.0255) H11D(0.0907) H11E(0.1404)
 H11F(0.1826) H12D(0.0639) H12E(0.1556) H12F(0.1002)
;