Improving intramolecular hydroamination Rh(i) and Ir(i) catalysts through targeted ligand modification
Beeren, Sophie R.; Dabb, Serin L.; Edwards, Gavin; Smith, Matthew K.; Willis, Anthony C.; Messerle, Barbara A.; New Journal of Chemistry 34 (2010) 1200–; doi:10.1039/b9nj00759h

data_7053430
_publ_section_title
;
 Improving intramolecular hydroamination Rh(i) and Ir(i) catalysts through
 targeted ligand modification
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1200
_journal_paper_doi               10.1039/b9nj00759h
_journal_volume                  34
_journal_year                    2010
_chemical_compound_source        ' from UNSW '
_chemical_formula_moiety         'C23 H17 F3 N2 O4 P Rh S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C23.5 H18 Cl F3 N2 O4 P Rh S'
_chemical_formula_weight         650.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-06-27
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2007-06-27 - Report on C23.50 H18 Cl F3 N2 O4 P Rh S
by Anthony C. Willis
for Serin Dabb and Barbara Messerle (UNSW)

2007-06-27 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 100.3725(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5808(1)
_cell_length_b                   20.0102(3)
_cell_length_c                   12.2975(2)
_cell_measurement_reflns_used    35612
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2561.13(6)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52493
_diffrn_reflns_theta_full        27.477
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.552
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9769
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5838
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001102
_refine_ls_structure_factor_coef Fsqd
_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:
10.8 16.0 8.35 2.66 0.0970
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0887
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0887
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3975
_reflns_number_total             5855
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.32
_oxford_diffrn_Wilson_scale      32.40
_oxford_refine_ls_scale          0.18675(8)
_oxford_structure_analysis_title '6270851 nsw0705'
_cod_data_source_file            b9nj00759h.txt
_cod_data_source_block           nsw0705a
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value ' not measured ' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C23.50 H18 Cl F3 N2 O4 P Rh S'
_cod_database_code               7053430