Synthesis of New Chiral Bidentate Isonitrile‒Acyclic Diaminocarbene Palladium(II) Compounds and Their Catalytic Activity
Knorn, Matthias; Lutsker, Eugen; Reiser, Oliver; Organometallics 34 (2015) 4515–; doi:10.1021/acs.organomet.5b00516

data_4086258
_publ_section_title
;
 Synthesis of New Chiral Bidentate Isonitrile--Acyclic Diaminocarbene
 Palladium(II) Compounds and Their Catalytic Activity
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4515
_journal_paper_doi               10.1021/acs.organomet.5b00516
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H38 Cl2 N3 O3 P Pd'
_chemical_formula_sum            'C24 H38 Cl2 N3 O3 P Pd'
_chemical_formula_weight         624.84
_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   mixed
_audit_creation_date             2015-04-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.91450(9)
_cell_length_b                   18.83710(10)
_cell_length_c                   24.40150(13)
_cell_measurement_temperature    123
_cell_volume                     5936.20(6)
_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      123.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41098
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.636
_diffrn_reflns_theta_max         66.636
_diffrn_reflns_theta_min         3.623
_exptl_absorpt_coefficient_mu    7.436
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.198
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       prism
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.2956
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.0644
_refine_diff_density_max         0.633
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 4340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.780
_reflns_friedel_fraction_full    0.960
_reflns_friedel_fraction_max     0.960
_reflns_number_gt                10116
_reflns_number_total             10287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00516_si_002.cif
_cod_data_source_block           l170
_cod_original_cell_volume        5936.19(6)
_cod_database_code               4086258
_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) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C15(H15), C26(H26), C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C31(H31A,H31B), C38(H38A,H38B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B)
2.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
2.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37)
;
_shelx_res_checksum              95372
_shelx_hkl_checksum              60179
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments CryoJet'
_olex2_submission_original_sample_id 'Knorn MK-111.1.Pyr'
_olex2_submission_special_instructions 'No special instructions were received'