A Readily Accessible Chiral NNN Pincer Ligand with a Pyrrole Backbone and Its Ni(II) Chemistry: Syntheses, Structural Chemistry, and Bond Activations.
Wenz, Jan; Kochan, Alexander; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 56 (2017) 3631–3643; doi:10.1021/acs.inorgchem.7b00077

data_4345583
_publ_section_title
;
 A Readily Accessible Chiral NNN Pincer Ligand with a Pyrrole Backbone and
 Its Ni(II) Chemistry: Syntheses, Structural Chemistry, and Bond
 Activations.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3631
_journal_page_last               3643
_journal_paper_doi               10.1021/acs.inorgchem.7b00077
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H45 N3 Ni O2 Si'
_chemical_formula_sum            'C26 H45 N3 Ni O2 Si'
_chemical_formula_weight         518.45
_chemical_properties_physical    air-sensitive
_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_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_jw27
_audit_creation_date             2016-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
'26.02.2016 13:40:48 CET UTC+01:00  encif 1.38'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.44998(17)
_cell_length_b                   14.0215(2)
_cell_length_c                   17.5861(3)
_cell_measurement_reflns_used    26964
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      31.5760
_cell_measurement_theta_min      3.2600
_cell_volume                     2823.38(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      perfluoro
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      1.00  99.00   0.50   15.00    --   26.87  38.00  90.00  196
  2  \w      6.00  96.00   0.50   15.00    --   26.87  57.00 -60.00  180
  3  \w    -20.00  69.00   0.50   15.00    --   26.87 -99.00  60.00  178
  4  \w    -46.00  52.00   0.50   15.00    --   26.87 -38.00 150.00  196
  5  \w     -3.00  97.00   0.50   15.00    --   26.87  77.00  90.00  200
  6  \w     -3.00  97.00   0.50   15.00    --   26.87  77.00 -30.00  200
  7  \w     -3.00  97.00   0.50   15.00    --   26.87  77.00-120.00  200
  8  \w    -20.00  69.00   0.50   15.00    --   26.87 -99.00 -90.00  178
  9  \w    -20.00  69.00   0.50   15.00    --   26.87 -99.00 120.00  178
 10  \w    -15.00  48.00   0.50   15.00    --   26.87 -57.00 -60.00  126
 11  \w     -2.00  32.00   0.50   15.00    --   26.87  77.00-180.00   68
 12  \w     68.00  97.00   0.50   15.00    --   26.87  77.00-180.00   58
 13  \w    -19.00  66.00   0.50   15.00    --   26.87 -99.00 150.00  170
 14  \w      9.00  59.00   0.50   15.00    --   26.87  77.00   0.00  100
 15  \w    -18.00  10.00   0.50   15.00    --   26.87 -99.00 -30.00   56
 16  \w      3.00  75.00   0.50   15.00    --   26.87  38.00-150.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0200075000
_diffrn_orient_matrix_UB_12      -0.0291960000
_diffrn_orient_matrix_UB_13      -0.0302738000
_diffrn_orient_matrix_UB_21      0.0232111000
_diffrn_orient_matrix_UB_22      0.0328988000
_diffrn_orient_matrix_UB_23      -0.0266447000
_diffrn_orient_matrix_UB_31      0.0538148000
_diffrn_orient_matrix_UB_32      -0.0250253000
_diffrn_orient_matrix_UB_33      0.0002806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            87148
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.388
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 3595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0287P)^2^+0.6040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                8910
_reflns_number_total             9760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00077_si_002.cif
_cod_data_source_block           ga_jw27
_cod_original_cell_volume        2823.37(7)
_cod_database_code               4345583
_audit_block_refno               2663
_audit_block_usercomment         'jw441, irregular, yellow'
_chemical_oxdiff_formula         'C26 H45 N3 Si Ni O2'
_chemical_oxdiff_usercomment     'jw441, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.900
_reflns_odcompleteness_completeness 94.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.78
_shelxl_version_number           2014/7
_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 Ternary CH refined with riding coordinates:
 C1(H1), C12(H12), C13(H13), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              89516
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.799
_cell_oxdiff_length_a            11.4536(2)
_cell_oxdiff_length_b            14.0160(2)
_cell_oxdiff_length_c            17.5874(2)
_cell_oxdiff_angle_alpha         90.0076(11)
_cell_oxdiff_angle_beta          90.0543(13)
_cell_oxdiff_angle_gamma         90.0190(13)
_cell_oxdiff_volume              2823.37(7)
_cell_oxdiff_measurement_reflns_used 26964