[Cp(Ar)Ni{Ga(nacnac)}]: An Open-Shell Nickel(I) Complex Supported by a Gallium(I) Carbenoid (Cp(Ar) = C5(C6H4-4-Et)5, nacnac = HC[C(Me)N-(C6H3)-2,6-iPr2]2).
Chakraborty, Uttam; Mühldorf, Bernd; van Velzen, Niels J. C.; de Bruin, Bas; Harder, Sjoerd; Wolf, Robert; Inorganic chemistry 55 (2016) 3075–3078; doi:10.1021/acs.inorgchem.5b02979

data_4347292
_publ_section_title
;
 [Cp(Ar)Ni{Ga(nacnac)}]: An Open-Shell Nickel(I) Complex Supported by a
 Gallium(I) Carbenoid (Cp(Ar) = C5(C6H4-4-Et)5, nacnac =
 HC[C(Me)N-(C6H3)-2,6-iPr2]2).
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3075
_journal_page_last               3078
_journal_paper_doi               10.1021/acs.inorgchem.5b02979
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C74 H86 Ga N2 Ni'
_chemical_formula_sum            'C74 H86 Ga N2 Ni'
_chemical_formula_weight         1131.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9460(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.54658(18)
_cell_length_b                   11.25766(8)
_cell_length_c                   22.79169(15)
_cell_measurement_reflns_used    25590
_cell_measurement_temperature    124(1)
_cell_measurement_theta_max      65.7990
_cell_measurement_theta_min      4.3190
_cell_volume                     6221.57(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      124(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.986
_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    -27.00  68.00   0.50    7.50    --   39.03 -38.00  90.00  190
  2  \w     26.00 115.00   0.50    7.50    --   39.03  57.00-120.00  178
  3  \w     74.00 100.00   0.50   30.00    --   93.50 -86.00-102.73   52
  4  \w     37.00  63.00   0.50   30.00    --   93.50 -89.00 -20.62   52
  5  \w    101.00 133.00   0.50   30.00    --   93.50 -89.00 -20.62   64
  6  \w     39.00 144.00   0.50   30.00    --   93.50  18.00 -13.41  210
  7  \w    101.00 130.00   0.50   30.00    --   93.50  30.00   0.00   58
  8  \w     15.00  69.00   0.50   30.00    --   93.50 -30.00  90.00  108
  9  \w    100.00 125.00   0.50   30.00    --   93.50 -61.00  90.00   50
 10  \w     23.00  48.00   0.50   30.00    --   93.50 -30.00  60.00   50
 11  \w     28.00  68.00   0.50   30.00    --   93.50 -30.00 150.00   80
 12  \w     38.00  81.00   0.50   30.00    --   93.50 -61.00  60.00   86
 13  \w     87.00 123.00   0.50   30.00    --   93.50 -61.00  60.00   72
 14  \w     65.00 102.00   0.50   30.00    --   93.50  45.00  30.00   74
 15  \w     93.00 119.00   0.50   30.00    --   93.50 -61.00   0.00   52
 16  \w    133.00 159.00   0.50   30.00    --   93.50  45.00  30.00   52
 17  \w    133.00 159.00   0.50   30.00    --   93.50  15.00 -30.00   52
 18  \w     23.00  74.00   0.50   30.00    --   93.50 -61.00  90.00  102
 19  \w     41.00  74.00   0.50   30.00    --   93.50 -45.00 150.00   66
 20  \w     75.00 102.00   0.50   30.00    --   93.50  45.00 -90.00   54
 21  \w    131.00 157.00   0.50   30.00    --   93.50  45.00 -90.00   52
 22  \w     20.00  46.00   0.50   30.00    --   93.50 -61.00 120.00   52
 23  \w     76.00 125.00   0.50   30.00    --   93.50 -61.00 120.00   98
 24  \w     39.00  64.00   0.50   30.00    --   93.50 -30.00 120.00   50
 25  \w     11.00  37.00   0.50   30.00    --   93.50 -95.00 -90.00   52
 26  \w      9.00  52.00   0.50   30.00    --   93.50 -95.00 120.00   86
 27  \w     55.00  85.00   0.50   30.00    --   93.50 178.00  30.00   60
 28  \w      9.00  55.00   0.50   30.00    --   93.50 -15.00 -30.00   92
 29  \w    134.00 159.00   0.50   30.00    --   93.50 -15.00 -30.00   50
 30  \w     33.00  58.00   0.50   30.00    --   93.50 -61.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315140000
_diffrn_orient_matrix_UB_12      0.0204365000
_diffrn_orient_matrix_UB_13      -0.0525423000
_diffrn_orient_matrix_UB_21      0.0547471000
_diffrn_orient_matrix_UB_22      -0.0284051000
_diffrn_orient_matrix_UB_23      0.0404892000
_diffrn_orient_matrix_UB_31      -0.0068686000
_diffrn_orient_matrix_UB_32      -0.1322738000
_diffrn_orient_matrix_UB_33      -0.0168008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43685
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.021
_diffrn_reflns_theta_min         3.646
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+4.1823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9531
_reflns_number_total             10697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02979_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        6221.58(8)
_cod_database_code               4347292
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C74H86NiGaN2
_reflns_odcompleteness_completeness 96.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C37A) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: H36A(0.75) H36B(0.75) H36C(0.25) H36D(0.25) C37A(0.75) H37A(0.75)
 H37B(0.75) H37C(0.75) C37(0.25) H37D(0.25) H37E(0.25) H37F(0.25)
4.a Ternary CH refined with riding coordinates:
 C57(H57), C58(H58), C72(H72), C69(H69)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C12(H12A,H12B), C28(H28A,H28B), C20(H20A,H20B), C36(H36A,
 H36B), C36(H36C,H36D)
4.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C35(H35), C7(H7), C23(H23), C15(H15), C39(H39), C19(H19), C43(H43),
 C8(H8), C11(H11), C10(H10), C27(H27), C40(H40), C53(H53), C66(H66), C26(H26),
 C42(H42), C67(H67), C55(H55), C65(H65), C24(H24), C16(H16), C18(H18), C31(H31),
  C54(H54), C34(H34), C32(H32)
4.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C45(H45A,H45B,H45C), C74(H74A,H74B,
 H74C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C73(H73A,H73B,H73C), C71(H71A,
 H71B,H71C), C70(H70A,H70B,H70C), C60(H60A,H60B,H60C), C21(H21A,H21B,H21C),
 C59(H59A,H59B,H59C), C29(H29A,H29B,H29C), C13(H13A,H13B,H13C), C37A(H37A,H37B,
 H37C), C37(H37D,H37E,H37F)
;
_shelx_res_checksum              77639
_shelx_hkl_checksum              95052
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.819