Alkynyl-functionalized gold NHC complexes and their coinage metal clusters.
Kiefer, Claude; Bestgen, Sebastian; Gamer, Michael T.; Lebedkin, Sergei; Kappes, Manfred M.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13662–13670; doi:10.1039/c5dt02228b

data_7035581
_publ_section_title
;
 Alkynyl-functionalized gold NHC complexes and their coinage metal
 clusters.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13662
_journal_page_last               13670
_journal_paper_doi               10.1039/c5dt02228b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C32 H46 B2 N O P2 S Si Tb, C4 H8 O'
_chemical_formula_sum            'C36 H54 B2 N O2 P2 S Si Tb'
_chemical_formula_weight         835.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-23 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.657(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8355(3)
_cell_length_b                   11.4119(4)
_cell_length_c                   36.1580(11)
_cell_measurement_reflns_used    14280
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      1.87
_cell_volume                     4022.2(2)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1463
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            30568
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.104
_diffrn_reflns_theta_min         1.873
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  0.7386
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       needle
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7935
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0483P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4208
_reflns_number_total             7935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02228b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7035578--7035585.cif.'
_cod_database_code               7035581
_audit_block_doi                 10.5517/cc13y1tx
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2A-H2D = H2B-H2A = H2B-H2D = H2C-H2D = H2C-H2A = H2B-H2C
 1.7 with sigma of 0.02
 B2-H2A = B2-H2B = B2-H2D = B2-H2C
 1.05 with sigma of 0.02
 B1-H1D = B1-H1B = B1-H1C = B1-H1A
 1.05 with sigma of 0.02
 H1C-H1D = H1C-H1B = H1D-H1B = H1C-H1A = H1B-H1A = H1D-H1A
 1.7 with sigma of 0.02
3. Rigid bond restraints
 C30, C31B, C31A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C34A) \\sim Ueq, Uanis(C34B) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
5. Others
 Sof(H30C)=Sof(H30D)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(H33C)=Sof(H33D)=Sof(H35C)=Sof(H35D)=1-FVAR(2)
 Sof(H33A)=Sof(H33B)=Sof(H35A)=Sof(H35B)=FVAR(2)
 Fixed Sof: C31A(0.5) H31A(0.5) H31B(0.5) C31B(0.5) H31C(0.5) H31D(0.5)
 C34A(0.33333) H34A(0.33333) H34B(0.33333) C34B(0.66667) H34C(0.66667)
 H34D(0.66667)
6.a Ternary CH refined with riding coordinates:
 C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30C,H30D), C30(H30A,H30B), C31A(H31A,H31B), C31B(H31C,
 H31D), C32(H32C,H32D), C32(H32A,H32B), C33(H33C,H33D), C33(H33A,H33B),
 C34A(H34A,H34B), C34B(H34C,H34D), C35(H35C,H35D), C35(H35A,H35B), C36(H36A,
 H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              88441
_olex2_submission_special_instructions 'No special instructions were received'