A Golden Ring: Molecular Gold Carbido Complexes
Elliot S. Borren; Anthony F. Hill; Rong Shang; Manab Sharma; Anthony C. Willis; Journal of the American Chemical Society 135 (2013) 4942–4945; doi:10.1021/ja400128h

data_4119539
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' afhill@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony F. Hill '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 A Golden Ring: Molecular Gold Carbido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4942
_journal_page_last               4945
_journal_paper_doi               10.1021/ja400128h
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        local
_chemical_formula_moiety         'C72 H88 Au4 B4 N24 O9 W4, H2 O'
_chemical_formula_sum            'C72 H90 Au4 B4 N24 O9 W4'
_chemical_formula_weight         3002.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_date             12-04-02
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
;
2012-03-30 - Report on C17 H12 N2 O
             by Anthony C. Willis
             for   Manab Sharma and Tony Hill

2012-03-30 - passes checkcif tests with minor warnings  
;
_cell_angle_alpha                89.6316(13)
_cell_angle_beta                 70.6096(13)
_cell_angle_gamma                85.4020(12)
_cell_formula_units_Z            2
_cell_length_a                   14.1428(4)
_cell_length_b                   19.4442(4)
_cell_length_c                   19.5444(3)
_cell_measurement_reflns_used    126189
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     5052.3(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Platon (Spek, 2008)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement
; 
CRYSTALS (Betteridge et al., 2003),
Platon (Spek, 2008)
;
_computing_structure_solution    'Superflip, Palatinus & Chapuis, 2007'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80085
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.701
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.374
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_description       plate
_exptl_crystal_F_000             2784.000
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
;
_refine_diff_density_max         3.43
_refine_diff_density_min         -2.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9588
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         17730
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.0242350
_refine_ls_shift/su_mean         0.0007696
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 132. 215. 129. 52.5 12.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2197
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2196
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                13065
_reflns_number_total             17735
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.27
_oxford_diffrn_Wilson_scale      150.18
_oxford_refine_ls_r_factor_ref   0.0959
_oxford_refine_ls_scale          0.14428(8)
_oxford_reflns_number_all        17732
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '3271744 tony'
_cod_data_source_file            ja400128h_si_001.cif
_cod_data_source_block           manab_manWCAu
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4119539
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, AU(1,U'S) UNTIL W(7) 
CONT O(25,U[ISO]) UNTIL B(101) 
CONT N(14,OCC) N(15,OCC) N(114,OCC) N(115,OCC) 
CONT C(20,OCC) UNTIL C(24) C(120,OCC) UNTIL C(124) 
CONT B(1,OCC) B(101,OCC) 
EQUIV N(14,OCC) N(15,OCC) N(114,OCC) N(115,OCC) 
CONT C(20,OCC) UNTIL C(24) C(120,OCC) UNTIL C(124) 
CONT B(1,OCC) B(101,OCC) 
WEIGHT -1  N(114,OCC) N(115,OCC) C(120,OCC) UNTIL C(124) 
CONT B(101,OCC) 
SUMFIX ELEMENT SCALES 
RIDE C ( 11,X'S) H( 111,X'S) 
RIDE C ( 13,X'S) H( 131,X'S) H( 132,X'S) H( 133,X'S) 
RIDE C ( 14,X'S) H( 141,X'S) H( 142,X'S) H( 143,X'S) 
RIDE C ( 16,X'S) H( 161,X'S) 
RIDE C ( 18,X'S) H( 181,X'S) H( 182,X'S) H( 183,X'S) 
RIDE C ( 19,X'S) H( 191,X'S) H( 192,X'S) H( 193,X'S) 
RIDE C ( 21,X'S) H( 211,X'S) 
RIDE C ( 23,X'S) H( 231,X'S) H( 232,X'S) H( 233,X'S) 
RIDE C ( 24,X'S) H( 241,X'S) H( 242,X'S) H( 243,X'S) 
RIDE C ( 121,X'S) H( 1211,X'S) 
RIDE C ( 123,X'S) H( 1231,X'S) H( 1232,X'S) H( 1233,X'S) 
RIDE C ( 124,X'S) H( 1241,X'S) H( 1242,X'S) H( 1243,X'S) 
RIDE C ( 31,X'S) H( 311,X'S) 
RIDE C ( 33,X'S) H( 331,X'S) H( 332,X'S) H( 333,X'S) 
RIDE C ( 34,X'S) H( 341,X'S) H( 342,X'S) H( 343,X'S) 
RIDE C ( 36,X'S) H( 361,X'S) 
RIDE C ( 38,X'S) H( 381,X'S) H( 382,X'S) H( 383,X'S) 
RIDE C ( 39,X'S) H( 391,X'S) H( 392,X'S) H( 393,X'S) 
RIDE C ( 41,X'S) H( 411,X'S) 
RIDE C ( 53,X'S) H( 531,X'S) H( 532,X'S) H( 533,X'S) 
RIDE C ( 54,X'S) H( 541,X'S) H( 542,X'S) H( 543,X'S) 
RIDE C ( 56,X'S) H( 561,X'S) 
RIDE C ( 58,X'S) H( 581,X'S) H( 582,X'S) H( 583,X'S) 
RIDE C ( 59,X'S) H( 591,X'S) H( 592,X'S) H( 593,X'S) 
RIDE C ( 61,X'S) H( 611,X'S) 
RIDE C ( 63,X'S) H( 631,X'S) H( 632,X'S) H( 633,X'S) 
RIDE C ( 64,X'S) H( 641,X'S) H( 642,X'S) H( 643,X'S) 
RIDE C ( 71,X'S) H( 711,X'S) 
RIDE C ( 73,X'S) H( 731,X'S) H( 732,X'S) H( 733,X'S) 
RIDE C ( 74,X'S) H( 741,X'S) H( 742,X'S) H( 743,X'S) 
RIDE C ( 76,X'S) H( 761,X'S) 
RIDE C ( 78,X'S) H( 781,X'S) H( 782,X'S) H( 783,X'S) 
RIDE C ( 79,X'S) H( 791,X'S) H( 792,X'S) H( 793,X'S) 
RIDE C ( 81,X'S) H( 811,X'S) 
RIDE C ( 83,X'S) H( 831,X'S) H( 832,X'S) H( 833,X'S) 
RIDE C ( 84,X'S) H( 841,X'S) H( 842,X'S) H( 843,X'S) 
RIDE B(1,X'S) H(11,X'S) 
RIDE B(101,X'S) H(1011,X'S) 
RIDE B(3,X'S) H(31,X'S) 
RIDE B(5,X'S) H(51,X'S) 
RIDE B(7,X'S) H(71,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
PLANAR N(10) N(11) C(10) UNTIL C(14) B(1) 
DIST 1.57, 0.02 = B(1) TO N(11) 
DIST 1.37, 0.02 = N(11) TO N(10) 
DIST 1.36, 0.02 = N(10) TO C(10), N(11) TO C(12) 
DIST 1.38, 0.02 = C(12) TO C(11), C(11) TO C(10) 
DIST 1.54, 0.02 = C(10) TO C(13), C(12) TO C(14) 
ANGLE 129, 3.0 = B(1) TO N(11) TO C(12) 
ANGLE 120, 3.0 = B(1) TO N(11) TO N(10) 
ANGLE 111, 3.0 = N(10) TO N(11) TO C(12) 
ANGLE 109, 3.0 = N(11) TO C(12) TO C(11), C(11) TO C(10) TO N(10) 
ANGLE 122, 3.0 = N(11) TO C(12) TO C(14), N(10) TO C(10) TO C(13) 
ANGLE 129, 3.0 = C(14) TO C(12) TO C(11), C(13) TO C(10) TO C(11) 
ANGLE 107, 3.0 = C(12) TO C(11) TO C(10) 
ANGLE 106, 3.0 = N(11) TO N(10) TO C(10) 
REM 
REM MOLECULE 2 - DISORDER PART 1 
PLANAR N(14) N(15) C(20) UNTIL C(24) B(1) 
DIST 1.57, 0.02 = B(1) TO N(15) 
DIST 1.37, 0.02 = N(14) TO N(15) 
DIST 1.36, 0.02 = N(15) TO C(22), N(14) TO C(20) 
DIST 1.38, 0.02 = C(22) TO C(21), C(21) TO C(20) 
DIST 1.54, 0.02 = C(20) TO C(23), C(22) TO C(24) 
ANGLE 129, 3.0 = B(1) TO N(15) TO C(22) 
ANGLE 120, 3.0 = B(1) TO N(15) TO N(14) 
ANGLE 111, 3.0 = N(14) TO N(15) TO C(22) 
ANGLE 109, 3.0 = N(15) TO C(22) TO C(21), C(21) TO C(20) TO N(14) 
ANGLE 122, 3.0 = N(15) TO C(22) TO C(24), N(14) TO C(20) TO C(23) 
ANGLE 129, 3.0 = C(24) TO C(22) TO C(21), C(23) TO C(20) TO C(21) 
ANGLE 107, 3.0 = C(22) TO C(21) TO C(20) 
ANGLE 106, 3.0 = N(15) TO N(14) TO C(20) 
REM 
REM MOLECULE 2 - DISORDER PART 2 
PLANAR N(114) N(115) C(120) UNTIL C(124) B(101) 
DIST 1.57, 0.02 = B(101) TO N(115) 
DIST 1.37, 0.02 = N(114) TO N(115) 
DIST 1.36, 0.02 = N(115) TO C(122), N(114) TO C(120) 
DIST 1.38, 0.02 = C(122) TO C(121), C(121) TO C(120) 
DIST 1.54, 0.02 = C(120) TO C(123), C(122) TO C(124) 
ANGLE 129, 3.0 = B(101) TO N(115) TO C(122) 
ANGLE 120, 3.0 = B(101) TO N(115) TO N(114) 
ANGLE 111, 3.0 = N(114) TO N(115) TO C(122) 
ANGLE 109, 3.0 = N(115) TO C(122) TO C(121), C(121) TO C(120) TO N(114) 
ANGLE 122, 3.0 = N(115) TO C(122) TO C(124), N(114) TO C(120) TO C(123) 
ANGLE 129, 3.0 = C(124) TO C(122) TO C(121), C(123) TO C(120) TO C(121) 
ANGLE 107, 3.0 = C(122) TO C(121) TO C(120) 
ANGLE 106, 3.0 = N(115) TO N(114) TO C(120) 
REM 
REM MOLECULE 3 
PLANAR 0.05 N(12) N(12) C(15) UNTIL C(19) B(1) 
DIST 1.57, 0.02 = B(1) TO N(13) 
DIST 1.37, 0.02 = N(13) TO N(12) 
DIST 1.36, 0.02 = N(12) TO C(15), N(13) TO C(17) 
DIST 1.38, 0.02 = C(17) TO C(16), C(16) TO C(15) 
DIST 1.54, 0.02 = C(15) TO C(18), C(17) TO C(19) 
ANGLE 129, 3.0 = B(1) TO N(13) TO C(17) 
ANGLE 120, 3.0 = B(1) TO N(13) TO N(12) 
ANGLE 111, 3.0 = N(12) TO N(13) TO C(17) 
ANGLE 109, 3.0 = N(13) TO C(17) TO C(16), C(16) TO C(15) TO N(12) 
ANGLE 122, 3.0 = N(13) TO C(17) TO C(19), N(12) TO C(15) TO C(18) 
ANGLE 129, 3.0 = C(19) TO C(17) TO C(16), C(18) TO C(15) TO C(16) 
ANGLE 107, 3.0 = C(17) TO C(16) TO C(15) 
ANGLE 106, 3.0 = N(13) TO N(12) TO C(15) 
REM 
LIMIT .0001 O(102,U[ISO]) 
LIMIT .0001 O(102,X) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;