1,1-P‒OP Ligands with P-Stereogenic Phosphino Groups in Asymmetric Hydrogenations and Hydroformylations
Lao, Joan R.; Benet-Buchholz, J.; Vidal-Ferran, Anton; Organometallics 33 (2014) 2960–; doi:10.1021/om500378b

data_4083556
_publ_section_title
;
 1,1-P--OP Ligands with P-Stereogenic Phosphino Groups in Asymmetric
 Hydrogenations and Hydroformylations
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2960
_journal_paper_doi               10.1021/om500378b
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C48.5 H57 B O3 P2'
_chemical_formula_weight         760.69
_chemical_name_systematic
;
 ?
;
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_space_group_name_Hall           'P 1'
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_symmetry_space_group_name_Hall  'P 1'
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_cell_angle_beta                 90.306(4)
_cell_angle_gamma                105.477(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9989(12)
_cell_length_b                   11.2875(12)
_cell_length_c                   18.3289(19)
_cell_measurement_reflns_used    9186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.31
_cell_volume                     2125.3(4)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
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_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.982
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_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_point_group_measured_fraction_full 0.719
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_diffrn_reflns_theta_full        25.000
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_diffrn_source                   'Rotating anode X-ray tube'
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_diffrn_source_power             50
_diffrn_source_size              '0.3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
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_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       prism
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
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_refine_diff_density_max         0.505
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 4026 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         17554
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0591P)^2^+0.4187P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15827
_reflns_number_total             17554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500378b_si_002.cif
_cod_data_source_block           JL085b_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083555--4083557.cif.
;
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C48.50 H57 B O3 P2'
_cod_database_code               4083556
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2012-9
_shelx_res_checksum              30953
_shelx_hkl_checksum              60444