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_7029398
_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         'C34 H46 N3 Ni, F6 P'
_chemical_formula_sum            'C34 H46 F6 N3 Ni P'
_chemical_formula_weight         700.42
_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             2013-05-18
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                75.910(5)
_cell_angle_beta                 86.934(5)
_cell_angle_gamma                81.371(5)
_cell_formula_units_Z            4
_cell_length_a                   10.3048(8)
_cell_length_b                   18.3915(10)
_cell_length_c                   19.1066(10)
_cell_measurement_reflns_used    16092
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4417
_cell_measurement_theta_min      3.2916
_cell_volume                     3471.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      100(2)
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -91.00  -13.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  151.0000 -172.0000 78

  2 omega  -90.00  -13.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  150.0000   26.0000 77

  3 omega  -40.00   60.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840   38.0000 -150.0000 100

  4 omega  -92.00  -10.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  -38.0000 -120.0000 82

  5 omega  -87.00    6.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  -38.0000  150.0000 93

  6 omega  -90.00   13.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  -57.0000   60.0000 103

  7 omega  -60.00   47.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6965  -77.0000    0.0000 107

  8 omega  -16.00   75.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6965   77.0000    0.0000 91

  9 omega  -95.00  -31.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3840  -77.0000    0.0000 64

 10 omega  -73.00    4.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2278  124.0000  150.0000 77

 11 omega  -77.00   -1.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2278  130.0000   -4.0000 76

 12 omega  -90.00  -13.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2278  151.0000  -97.0000 77

 13 omega  -77.00   -4.00   1.0000   86.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2278  131.0000  -30.0000 73
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0110996000
_diffrn_orient_matrix_UB_12      -0.0247269000
_diffrn_orient_matrix_UB_13      0.0338710000
_diffrn_orient_matrix_UB_21      0.0197157000
_diffrn_orient_matrix_UB_22      -0.0316461000
_diffrn_orient_matrix_UB_23      -0.0150904000
_diffrn_orient_matrix_UB_31      0.0658528000
_diffrn_orient_matrix_UB_32      -0.0007018000
_diffrn_orient_matrix_UB_33      0.0095108000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97217
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         17567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0459P)^2^+3.1382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13845
_reflns_number_total             17567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53352b2.cif
_cod_data_source_block           2c
_cod_original_cell_volume        3471.8(4)
_cod_database_code               7029398
_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:
 C65(H65), C68(H68), C85(H85), C88(H88), C15(H15), C18(H18), C35(H35), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C52(H52), C51(H51), C55(H55), C54(H54), C61(H61), C62(H62),
 C63(H63), C81(H81), C82(H82), C83(H83), C3(H3), C4(H4), C5(H5), C1(H1), C2(H2),
  C11(H11), C12(H12), C13(H13), C31(H31), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C), C92(H92A,H92B,H92C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;