Anion exchange in [Ni(η(5)-C5H4R)(Cl)(NHC)]. Counterion effect on the structure and catalytic activity.
Buchowicz, Włodzimierz; Banach, Lukasz; Conder, Joanna; Guńka, Piotr A; Kubicki, Dominik; Buchalski, Piotr; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5847–5857; doi:10.1039/c3dt53352b

data_7029400
_publ_section_title
;
 Anion exchange in [Ni(\h(5)-C5H4R)(Cl)(NHC)]. Counterion effect on the
 structure and catalytic activity.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5847
_journal_page_last               5857
_journal_paper_doi               10.1039/c3dt53352b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H32 N3 Ni, N O3'
_chemical_formula_sum            'C28 H32 N4 Ni O3'
_chemical_formula_weight         531.28
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-23
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                89.233(3)
_cell_angle_beta                 80.886(3)
_cell_angle_gamma                85.015(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5478(3)
_cell_length_b                   8.8564(3)
_cell_length_c                   17.8908(5)
_cell_measurement_reflns_used    7642
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6410
_cell_measurement_theta_min      3.6880
_cell_volume                     1332.23(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.8877
_diffrn_measurement_details
;
  1 omega  -98.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6509  -77.0000 -180.0000 107

  2 omega   -9.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6509   57.0000  -60.0000 59

  3 omega  -27.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6509   38.0000  150.0000 30

  4 omega  -91.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6509  -77.0000   30.0000 104

  5 omega   56.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9634  179.0000   30.0000 54

  6 omega  -62.00  -37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9634  -19.0000  -60.0000 25

  7 omega   37.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9634  -99.0000  150.0000 25

  8 omega  -48.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9634  -38.0000 -120.0000 42

  9 omega  -95.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  153.0000  125.0889 81

 10 omega  -82.00  -55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  -57.0000  -30.0000 27

 11 omega  -80.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  179.0000   30.0000 48

 12 omega  -93.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  -57.0000  -90.0000 81

 13 omega  -44.00   56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946   38.0000   60.0000 100

 14 omega  -97.00  -58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4946  155.0000    8.4257 39
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0107328000
_diffrn_orient_matrix_UB_12      -0.0800319000
_diffrn_orient_matrix_UB_13      0.0030833000
_diffrn_orient_matrix_UB_21      0.0762963000
_diffrn_orient_matrix_UB_22      0.0058277000
_diffrn_orient_matrix_UB_23      0.0100062000
_diffrn_orient_matrix_UB_31      -0.0343400000
_diffrn_orient_matrix_UB_32      0.0048931000
_diffrn_orient_matrix_UB_33      0.0387637000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26005
_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         27.500
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0483P)^2^+0.4188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5156
_reflns_number_total             6117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53352b2.cif
_cod_data_source_block           2j
_cod_original_cell_volume        1332.22(7)
_cod_database_code               7029400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C13(H13),
 C21(H21), C23(H23)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C)
;