Conformational Preferences Driven by the C-Methyl Substituent in Chelated o-Diphenylphosphino-α-methyl-N,N-dimethylbenzylamine Rhodium Complexes
M. Aránzazu Alonso; Juan A. Casares; Pablo Espinet; Katerina Soulantica; A. Guy Orpen; Hirihattaya Phetmung; Inorganic Chemistry 42 (2003) 3856–3864; doi:10.1021/ic034117a

data_4313774
_publ_section_title
;
 Conformational Preferences Driven by the C-Methyl Substituent in Chelated
 o-Diphenylphosphino-\a-methyl-N,N-dimethylbenzylamine Rhodium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3856
_journal_page_last               3864
_journal_paper_doi               10.1021/ic034117a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C45 H57 B2 F12 N3 O2 P Rh'
_chemical_formula_weight         1055.44
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.742(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0548(11)
_cell_length_b                   16.139(2)
_cell_length_c                   12.1804(10)
_cell_measurement_reflns_used    10196
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     2328.2(4)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART area detector'
_diffrn_measurement_method       'narrow frame \w scans'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14885
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.97864
_exptl_absorpt_correction_T_min  0.912884
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10196
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_obs          0.0310
_refine_ls_shift/esd_max         -0.129
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0688
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          9090
_reflns_number_total             10196
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034117asi20030409_082812.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core 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 the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313774