[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_4347293
_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 Br Ga N2 Ni'
_chemical_formula_sum            'C74 H86 Br Ga N2 Ni'
_chemical_formula_weight         1211.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7389(19)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.8919(4)
_cell_length_b                   22.8702(4)
_cell_length_c                   38.3227(7)
_cell_measurement_reflns_used    60507
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.6640
_cell_measurement_theta_min      3.9170
_cell_volume                     20749.3(6)
_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      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -116.00 -26.00   0.50   10.00    --  -40.71 -37.00 -30.00  180
  2  \w     25.00  66.00   0.50   10.00    --   40.71 -57.00 -30.00   82
  3  \w      4.00  93.00   0.50   10.00    --   40.71-125.00 -60.00  178
  4  \w     32.00  69.00   0.50   30.00    --  106.98 -30.00-120.00   74
  5  \w     33.00 121.00   0.50   30.00    --  106.98-124.00  92.00  176
  6  \w     44.00 103.00   0.50   30.00    --  106.98 -94.00 -30.00  118
  7  \w     42.00  76.00   0.50   30.00    --  106.98 -45.00  30.00   68
  8  \w     36.00  65.00   0.50   30.00    --  106.98 -30.00-150.00   58
  9  \w     36.00  65.00   0.50   30.00    --  106.98 -30.00 -90.00   58
 10  \w     42.00  68.00   0.50   30.00    --  106.98 -30.00-180.00   52
 11  \w     35.00 118.00   0.50   30.00    --  106.98-125.00 -90.00  166
 12  \w     42.00  68.00   0.50   30.00    --  106.98 -30.00  90.00   52
 13  \w     43.00 102.00   0.50   30.00    --  106.98 -94.00 -90.00  118
 14  \w     80.00 154.00   0.50   30.00    --  106.98  30.00  30.00  148
 15  \w   -127.00 -41.00   0.50   10.00    --  -40.71-172.00  37.00  172
 16  \w   -115.00 -11.00   0.50   10.00    --  -40.71 -57.00  60.00  208
 17  \w   -115.00 -11.00   0.50   10.00    --  -40.71 -57.00 150.00  208
 18  \w   -117.00 -14.00   0.50   10.00    --  -40.71 -37.00-120.00  206
 19  \w     76.00 158.00   0.50   30.00    --  106.98  30.00 -60.00  164
 20  \w     76.00 158.00   0.50   30.00    --  106.98  30.00 120.00  164
 21  \w     76.00 158.00   0.50   30.00    --  106.98  30.00-150.00  164
 22  \w     29.00  54.00   0.50   30.00    --  106.98 -30.00 -60.00   50
 23  \w     32.00  77.00   0.50   30.00    --  106.98 -45.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180038000
_diffrn_orient_matrix_UB_12      -0.0451701000
_diffrn_orient_matrix_UB_13      0.0292159000
_diffrn_orient_matrix_UB_21      0.0095392000
_diffrn_orient_matrix_UB_22      0.0496447000
_diffrn_orient_matrix_UB_23      0.0272997000
_diffrn_orient_matrix_UB_31      -0.0617827000
_diffrn_orient_matrix_UB_32      -0.0056320000
_diffrn_orient_matrix_UB_33      0.0069574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            173427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.021
_diffrn_reflns_theta_min         3.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             7656
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2179
_refine_ls_number_reflns         41200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+21.3126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32975
_reflns_number_total             41200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02979_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;

2020-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C222 H258 Br3 Ga3 N6 Ni3'
_cod_original_formula_weight         3635.35
_cod_original_formula_moiety         '3(C74 H86 Br Ga N2 Ni)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        20749.3(7)
_cod_database_code               4347293
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C74H86NiN2GaBr
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C364(H364), C357(H357), C366(H366), C360(H360), C35(H35), C43(H43), C32(H32),
 C46(H46), C198(H198), C197(H197), C204(H204), C206(H206)
2.b Secondary CH2 refined with riding coordinates:
 C447(H44a,H44b), C448(H44c,H44d), C449(H44e,H44f), C445(H44g,H44h), C446(H44i,
 H44j), C127(H12a,H12b), C128(H12c,H12d), C130(H13g,H13h), C126(H12e,H12f),
 C129(H12g,H12h), C287(H28a,H28b), C286(H28c,H28d), C290(H29g,H29h), C288(H28e,
 H28f), C289(H28g,H28h)
2.c Aromatic/amide H refined with riding coordinates:
 C336(H336), C349(H349), C382(H382), C343(H343), C351(H351), C347(H347),
 C365(H365), C386(H386), C344(H344), C345(H345), C400(H400), C359(H359),
 C367(H367), C369(H369), C374(H374), C358(H358), C371(H371), C377(H377),
 C392(H392), C350(H350), C346(H346), C348(H348), C352(H352), C381(H381),
 C379(H379), C385(H385), C373(H373), C51(H51), C24(H24), C70(H70), C25(H25),
 C34(H34), C54(H54), C26(H26), C56(H56), C28(H28), C30(H30), C22(H22), C27(H27),
  C31(H31), C61(H61), C58(H58), C48(H48), C45(H45), C49(H49), C18(H18),
 C33(H33), C66(H66), C29(H29), C44(H44), C80(H80), C23(H23), C64(H64), C60(H60),
  C175(H175), C186(H186), C188(H188), C187(H187), C182(H182), C199(H199),
 C220(H220), C213(H213), C218(H218), C184(H184), C212(H212), C196(H196),
 C185(H185), C225(H225), C228(H228), C221(H221), C190(H190), C203(H203),
 C237(H237), C208(H208), C209(H209), C224(H224), C216(H216), C191(H191),
 C189(H189), C183(H183), C205(H205)
2.d Idealised Me refined as rotating group:
 C337(H33a,H33b,H33c), C397(H39a,H39b,H39c), C340(H34a,H34b,H34c), C389(H38a,
 H38b,H38c), C398(H39d,H39e,H39f), C402(H40a,H40b,H40c), C403(H40d,H40e,H40f),
 C450(H45a,H45b,H45c), C464(H46a,H46b,H46c), C461(H46d,H46e,H46f), C390(H39g,
 H39h,H39i), C321(H32a,H32b,H32c), C395(H39j,H39k,H39l), C453(H45d,H45e,H45f),
 C458(H45g,H45h,H45i), C143(H14a,H14b,H14c), C19(H19a,H19b,H19c), C67(H67a,H67b,
 H67c), C17(H17a,H17b,H17c), C74(H74a,H74b,H74c), C77(H77a,H77b,H77c),
 C131(H13a,H13b,H13c), C75(H75a,H75b,H75c), C136(H13d,H13e,H13f), C82(H82a,H82b,
 H82c), C139(H13i,H13j,H13k), C140(H14d,H14e,H14f), C69(H69a,H69b,H69c),
 C78(H78a,H78b,H78c), C84(H84a,H84b,H84c), C176(H17d,H17e,H17f), C233(H23a,H23b,
 H23c), C297(H29a,H29b,H29c), C242(H24a,H24b,H24c), C296(H29d,H29e,H29f),
 C239(H23d,H23e,H23f), C230(H23g,H23h,H23i), C240(H24d,H24e,H24f), C300(H30a,
 H30b,H30c), C293(H29i,H29j,H29k), C305(H30d,H30e,H30f), C234(H23j,H23k,H23l),
 C179(H17g,H17h,H17i), C231(H23m,H23n,H23o), C244(H24g,H24h,H24i)
;
_shelx_res_checksum              53981
_shelx_hkl_checksum              60423
_shelx_fab_checksum              95563
_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 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.739