A rhodium(i)-oxygen adduct as a selective catalyst for one-pot sequential alkyne dimerization-hydrothiolation tandem reactions.
Kleinhans, George; Guisado-Barrios, Gregorio; Liles, David C.; Bertrand, Guy; Bezuidenhout, Daniela I.; Chemical communications (Cambridge, England) 52 (2016) 3504–3507; doi:10.1039/c6cc00029k

data_7118619
_publ_section_title
;
 A rhodium(i)-oxygen adduct as a selective catalyst for one-pot sequential
 alkyne dimerization-hydrothiolation tandem reactions.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3504
_journal_page_last               3507
_journal_paper_doi               10.1039/c6cc00029k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C60 H69 N7, Cl, F6 P'
_chemical_formula_sum            'C60 H69 Cl F6 N7 P'
_chemical_formula_weight         1068.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-06 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.8560(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2214(4)
_cell_length_b                   24.0518(5)
_cell_length_c                   15.2494(3)
_cell_measurement_temperature    150.15
_cell_volume                     5630.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            198184
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.247
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    1.404
_exptl_crystal_colour            'dull whiteish white'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.261
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11093
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0538P)^2^+3.5232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10149
_reflns_number_total             11093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00029k2.cif
_cod_data_source_block           cu_gkle0113_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7118618--7118619.cif.'
_cod_database_code               7118619
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-F3A \\sim F1-F4A \\sim F1-F5A \\sim F1-F6A
 with sigma of 0.02
 F2-F3A \\sim F2-F4A \\sim F2-F5A \\sim F2-F6A
 with sigma of 0.02
3. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C18(H18), C20(H20), C43(H43), C37(H37), C28(H28), C30(H30),
 C58(H58), C56(H56), C47(H47), C49(H49)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C44(H44A,H44B,H44C), C42(H42A,
 H42B,H42C), C41(H41A,H41B,H41C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C60(H60A,H60B,
 H60C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_olex2_submission_special_instructions 'No special instructions were received'