Intermolecular Hydroalkoxylation of Terminal Alkynes Catalyzed by a Dipyrrinato Rhodium(I) Complex with Unusual Selectivity
Lam, Raphael H.; Walker, D. Barney; Tucker, Matthew H.; Gatus, Mark R. D.; Bhadbhade, Mohan; Messerle, Barbara A.; Organometallics 34 (2015) 4312–; doi:10.1021/acs.organomet.5b00561

data_4087744
_publ_section_title
;
 Intermolecular Hydroalkoxylation of Terminal Alkynes Catalyzed by a
 Dipyrrinato Rhodium(I) Complex with Unusual Selectivity
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4312
_journal_paper_doi               10.1021/acs.organomet.5b00561
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C17 H11 N2 O2 Rh'
_chemical_formula_weight         378.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.606(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4114(10)
_cell_length_b                   17.2847(10)
_cell_length_c                   6.5749(4)
_cell_measurement_reflns_used    5394
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.781
_cell_measurement_theta_min      3.286
_cell_volume                     1409.04(16)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9850
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         3.640
_diffrn_source                   'Incoatec I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       'Thick plates'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0144P)^2^+2.1888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1180
_reflns_number_total             1240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00561_si_002.cif
_cod_data_source_block           Cc_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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_sg_symbol_H-M      'C 2/c'
_cod_database_code               4087744
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-4
_shelx_res_checksum              59839
_shelx_hkl_checksum              71655