A one-step, modular route to optically-active diphos ligands
E. Louise Hazeland; Andy M. Chapman; Paul G. Pringle; Hazel A. Sparkes; Chem.Commun. 51 (2015) 10206–; doi:10.1039/C5cc03517A

data_7117294
_publ_section_title
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 A one-step, modular route to optically-active diphos ligands
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_journal_name_full               Chem.Commun.
_journal_page_first              10206
_journal_paper_doi               10.1039/C5cc03517A
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H48 P2 Rh, B F4'
_chemical_formula_sum            'C33 H48 B F4 P2 Rh'
_chemical_formula_weight         696.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_audit_creation_date             2015-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6347(3)
_cell_length_b                   29.6678(7)
_cell_length_c                   10.7567(3)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.38
_cell_volume                     3262.88(15)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            114262
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         1.373
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0552 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.9225.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.018(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         15088
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0264P)^2^+0.7712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14574
_reflns_number_total             15088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03517a2.cif
_cod_data_source_block           lh283
_cod_database_code               7117294
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.018(13) -0.018(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C5(H5), C2(H2), C35(H35), C38(H38)
3.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C32(H32A,H32B), C33(H33A,H33B), C4(H4A,H4B),
 C3(H3A,H3B), C1(H1A,H1B), C66(H66A,H66B), C61(H61A,H61B), C62(H62A,H62B),
 C65(H65A,H65B), C36(H36A,H36B), C37(H37A,H37B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C30(H30), C31(H31), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C59(H59),
 C60(H60), C63(H63), C64(H64), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C),
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              953
_shelx_hkl_checksum              999
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'