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_7029401
_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         'C26 H29 N3 Ni O3'
_chemical_formula_sum            'C26 H29 N3 Ni O3'
_chemical_formula_weight         490.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-24
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6218(3)
_cell_length_b                   12.2104(3)
_cell_length_c                   22.7534(4)
_cell_measurement_reflns_used    20918
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.1610
_cell_measurement_theta_min      3.8390
_cell_volume                     4895.83(17)
_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
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.8762
_diffrn_measurement_details
;
  1 omega  -84.00  -41.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4060  -57.0000   90.0000 86

  2 omega   56.00   81.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185  179.0000 -120.0000 50

  3 omega  -70.00  -33.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185  179.0000   60.0000 74

  4 omega  -65.00  -32.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185  179.0000  -60.0000 66

  5 omega  -70.00  -12.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185  -19.0000  150.0000 116

  6 omega -100.00  -32.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4060  179.0000  -30.0000 136

  7 omega  -45.00    7.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4060   77.0000 -150.0000 104

  8 omega  -22.00   90.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185   77.0000 -120.0000 224

  9 omega   56.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7185  179.0000   30.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120719000
_diffrn_orient_matrix_UB_12      -0.0013172000
_diffrn_orient_matrix_UB_13      0.0297278000
_diffrn_orient_matrix_UB_21      -0.0051745000
_diffrn_orient_matrix_UB_22      -0.0575176000
_diffrn_orient_matrix_UB_23      -0.0019827000
_diffrn_orient_matrix_UB_31      0.0380360000
_diffrn_orient_matrix_UB_32      -0.0082289000
_diffrn_orient_matrix_UB_33      0.0091494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53880
_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         26.498
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82955
_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            red
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+1.2997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.948
_reflns_number_gt                8723
_reflns_number_total             9968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53352b2.cif
_cod_data_source_block           3c
_cod_original_cell_volume        4895.80(16)
_cod_database_code               7029401
_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:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C41(H41), C43(H43), C51(H51), C53(H53), 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:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C)
;