Tris(alkyne) and Bis(alkyne) Complexes of Coinage Metals: Synthesis and Characterization of (cyclooctyne)3M+(M = Cu, Ag) and (cyclooctyne)2Au+and Coinage Metal (M = Cu, Ag, Au) Family Group Trends
Das, Animesh; Dash, Chandrakanta; Celik, Mehmet Ali; Yousufuddin, Muhammed; Frenking, Gernot; Dias, H. V. Rasika; Organometallics 32 (2013) 3135–; doi:10.1021/om400073a

data_4089412
_publ_section_title
;
 Tris(alkyne) and Bis(alkyne) Complexes of Coinage Metals: Synthesis and
 Characterization of (cyclooctyne)3M+(M = Cu, Ag) and (cyclooctyne)2Au+and
 Coinage Metal (M = Cu, Ag, Au) Family Group Trends
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3135
_journal_paper_doi               10.1021/om400073a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C24 H35 Cu F6 Sb'
_chemical_formula_weight         622.81
_chemical_name_common            '[(cyclooctyne)3Cu][SbF6]'
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.552(2)
_cell_length_b                   9.2415(9)
_cell_length_c                   25.094(2)
_cell_measurement_reflns_used    4220
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.90
_cell_volume                     4998.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34434
_diffrn_reflns_theta_full        24.46
_diffrn_reflns_theta_max         24.46
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.986
_exptl_absorpt_correction_T_max  0.9072
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.160
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+73.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2120
_reflns_number_gt                3159
_reflns_number_total             4133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400073a_si_002.cif
_cod_data_source_block           dias769a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4997.9(8)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4089412