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_7118618
_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         'C72 H90 N7 O2 Rh, 0(H-21474836.48)'
_chemical_formula_sum            'C72 H90 N7 O2 Rh'
_chemical_formula_weight         1188.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-25
_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                103.4480(14)
_cell_angle_beta                 97.0590(13)
_cell_angle_gamma                107.0370(13)
_cell_formula_units_Z            2
_cell_length_a                   10.8323(5)
_cell_length_b                   15.4988(8)
_cell_length_c                   24.8410(13)
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      150.15
_cell_volume                     3795.4(3)
_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 0.972
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II-ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84650
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.780
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    0.267
_exptl_crystal_colour            'dull brownish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.032
_platon_squeeze_details
;
;
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         14487
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0660
_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^)+(0.1073P)^2^+1.4192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9945
_reflns_number_total             14487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00029k2.cif
_cod_data_source_block           mo_gkle0089_0m_a
_cod_depositor_comments
'Adding full bibliography for 7118618--7118619.cif.'
_cod_database_code               7118618
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C47-C46
 1.512 with sigma of 0.02
 C47-C46
 1.512 with sigma of 0.02
 C47-C46
 1.512 with sigma of 0.02
 C24-C21
 1.5 with sigma of 0.02
3. Restrained angles
 C49-C17-C19
 fixed at 95 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: H15(0) H(0) C48(0.75) H48A(0.75) H48B(0.75) H48C(0.75) H46(0.75)
 H46A(0.25) C49(0.25) H49A(0.25) H49B(0.25) H49C(0.25)
6.a Ternary CH refined with riding coordinates:
 C43(H43), C31(H31), C34(H34), C59(H59), C56(H56), C68(H68), C71(H71),
 C46(H46), C46(H46A)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C8(H8), C6(H6), C41(H41), C40(H40), C39(H39),
 C27(H27), C28(H28), C29(H29), C54(H54), C53(H53), C52(H52), C66(H66), C65(H65),
  C64(H64)
6.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C61(H61A,H61B,H61C), C60(H60A,
 H60B,H60C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C72(H72A,H72B,H72C), C48(H48A,H48B,
 H48C), C32(H32A,H32B,H32C), C49(H49A,H49B,H49C), C20(H20A,H20B,H20C), C19(H19A,
 H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C22(H22A,H22B,H22C),
 C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'