Rhodium(i) complexes bearing N-donor ligands: catalytic activity towards intramolecular cyclization of alkynoic acids and ligand lability
Man, Bradley Y.-W.; Bhadbhade, Mohan; Messerle, Barbara A.; New Journal of Chemistry 35 (2011) 1730–; doi:10.1039/c1nj20094a

data_7052681
_publ_section_title
;
 Rhodium(i) complexes bearing N-donor ligands: catalytic activity
 towards intramolecular cyclization of alkynoic acids and ligand
 lability
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1730
_journal_paper_doi               10.1039/c1nj20094a
_journal_volume                  35
_journal_year                    2011
_chemical_formula_sum            'C48 H47 B N7 Rh'
_chemical_formula_weight         835.65
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_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                   14.7482(17)
_cell_length_b                   21.214(3)
_cell_length_c                   25.120(3)
_cell_measurement_reflns_used    368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.834
_cell_measurement_theta_min      2.868
_cell_volume                     7859.3(17)
_computing_cell_refinement
;
APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA)
;
_computing_data_collection
;
APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_data_reduction
;
APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_molecular_graphics    'SHELXTL-Plus. Sheldrick, G. M. (2008)'
_computing_structure_refinement  'SHELXL-97. Sheldrick, G. M. (2008)'
_computing_structure_solution    'SHELXS-97. Sheldrick, G. M. (2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.3321
_diffrn_reflns_av_sigmaI/netI    0.4435
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31399
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plates'
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6893
_refine_ls_number_restraints     550
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.3212
_refine_ls_R_factor_gt           0.0856
_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^)+(0.1000P)^2^+0.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.2637
_reflns_number_gt                1982
_reflns_number_total             6893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20094a.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7859.2(17)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7052681