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_7117295
_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         'C29 H32 Cl2 O2 P2 Pt, C H2 Cl2'
_chemical_formula_sum            'C30 H34 Cl4 O2 P2 Pt'
_chemical_formula_weight         825.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8749(6)
_cell_length_b                   10.7553(6)
_cell_length_c                   29.0217(18)
_cell_measurement_temperature    100(2)
_cell_volume                     3082.3(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            108079
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.654
_diffrn_reflns_theta_min         2.019
_exptl_absorpt_coefficient_mu    5.030
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0745 after correction.
The Ratio of minimum to maximum transmission is 0.9124.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2907 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0159
_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^)+(0.0157P)^2^+0.5920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0371
_reflns_Friedel_coverage         0.773
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                6840
_reflns_number_total             7145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03517a2.cif
_cod_data_source_block           lh120_patt
_cod_database_code               7117295
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C18(H18), C3(H3), C5(H5), C8(H8), C7(H7), C15(H15), C4(H4),
 C13(H13), C16(H16), C14(H14)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              12060
_shelx_hkl_checksum              32605
_olex2_submission_special_instructions 'No special instructions were received'