Investigation of ligand steric effects on a highly cis-selective Rh(i) cyclopropanation catalyst
Rosenberg, Marianne Lenes; Langseth, Eirin; Krivokapic, Alexander; Gupta, Nalinava Sen; Tilset, Mats; New Journal of Chemistry 35 (2011) 2306–; doi:10.1039/c1nj20343f

data_7052756
_publ_section_title
;
 Investigation of ligand steric effects on a highly cis-selective Rh(i)
 cyclopropanation catalyst
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2306
_journal_paper_doi               10.1039/c1nj20343f
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C24 H27 Cl N3 O Rh, C H2 Cl2'
_chemical_formula_sum            'C25 H29 Cl3 N3 O Rh'
_chemical_formula_weight         596.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 100.9510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1361(8)
_cell_length_b                   14.0517(11)
_cell_length_c                   17.3518(13)
_cell_measurement_reflns_used    6725
_cell_measurement_temperature    105
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.36
_cell_volume                     2665.8(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      105
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23563
_diffrn_reflns_theta_full        25.647
_diffrn_reflns_theta_max         28.817
_diffrn_reflns_theta_min         1.879
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4788
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.000733
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.117 0.309E-01 0.106E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0374
_refine_ls_wR_factor_gt          0.0270
_refine_ls_wR_factor_ref         0.0262
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                5031
_reflns_number_total             6344
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.29
_oxford_diffrn_Wilson_scale      137.00
_oxford_refine_ls_r_factor_ref   0.0255
_oxford_refine_ls_scale          0.09369(7)
_oxford_reflns_number_all        6320
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c1nj20343f.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C25 H29 Cl3 N3 O1 Rh1'
_cod_database_code               7052756