Oxidative addition of methylene chloride to Me-DuPhos complexes of palladium and rhodium
Scheetz, Perry M.; Blank, Natalia F.; Gibbons, Sarah K.; Glueck, David S.; Rheingold, Arnold L.; Inorganica Chimica Acta 483 (2018) 111–115; doi:10.1016/j.ica.2018.08.007

data_1563930
_publ_section_title
;
 Oxidative addition of methylene chloride to Me-DuPhos complexes of
 palladium and rhodium
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              111
_journal_page_last               115
_journal_paper_doi               10.1016/j.ica.2018.08.007
_journal_volume                  483
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H58 Cl4 P4 Rh2, 5(C H2 Cl2)'
_chemical_formula_sum            'C42 H68 Cl14 P4 Rh2'
_chemical_formula_weight         1398.96
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6298(6)
_cell_length_b                   20.0689(9)
_cell_length_c                   22.7254(9)
_cell_measurement_reflns_used    6477
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.256
_cell_measurement_theta_min      2.411
_cell_volume                     5760.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23784
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.434
_diffrn_reflns_theta_min         1.792
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.1336
_exptl_absorpt_correction_T_min  0.0974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.7290.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       needle
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 2616 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+8.2414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                7916
_reflns_number_total             10531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2018-483-111.cif
_cod_data_source_block           glu532
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_database_code               1563930
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl4A(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) H6AD(0.5) Cl5A(0.5)
 Cl1(0.5) Cl7A(0.5)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C13(H13), C21(H21), C24(H24), C28(H28), C4AA(H4AA)
3.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C5(H5A,H5B), C11(H11A,H11B), C12(H12A,H12B),
  C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B), C30(H30A,H30B), C31(H31A,
 H31B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C6AA(H6AA,H6AB),
 C6AA(H6AC,H6AD)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C17(H17), C18(H18), C19(H19), C34(H34), C2AA(H2AA),
 C3AA(H3AA)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              71193
_shelx_hkl_checksum              17116
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'