Dispersion Force Stabilized Two-Coordinate Transition Metal-Amido Complexes of the -N(SiMe3)Dipp (Dipp = C6H3-2,6-Pri2) Ligand: Structural, Spectroscopic, Magnetic, and Computational Studies
Chun-Yi Lin; Jing-Dong Guo; James C. Fettinger; Shigeru Nagase; Fernande Grandjean; Gary J. Long; Nicholas F. Chilton; Philip P. Power; Inorganic Chemistry 52 (2013) 13584–13593; doi:10.1021/ic402105m

data_4336876
_publ_section_title
;
 Dispersion Force Stabilized Two-Coordinate Transition Metal-Amido
 Complexes of the -N(SiMe3)Dipp (Dipp = C6H3-2,6-Pri2) Ligand: Structural,
 Spectroscopic, Magnetic, and Computational Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13584
_journal_page_last               13593
_journal_paper_doi               10.1021/ic402105m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C64 H108 Cr4 N4 O Si4'
_chemical_formula_sum            'C64 H108 Cr4 N4 O Si4'
_chemical_formula_weight         1269.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-02
_audit_creation_method
; 
  Olex2 1.2 
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466) 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5098(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2421(3)
_cell_length_b                   16.2208(5)
_cell_length_c                   40.7752(13)
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      3.26
_cell_volume                     6753.2(4)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_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
; 
XL, G.M. Sheldrick, Acta Cryst. 
(2008). A64, 112-122 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            49668
_diffrn_reflns_theta_full        70.08
_diffrn_reflns_theta_max         70.08
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.154
_exptl_absorpt_correction_T_max  0.3724
_exptl_absorpt_correction_T_min  0.1600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       Block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         12744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+8.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                12374
_reflns_number_total             12744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402105m_si_002_4.cif
_cod_data_source_block           cyl018
_cod_database_code               4336876
_cod_database_fobs_code          4336876
_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: 
 C32(H32A), C10(H10), C7(H7), C13(H13A), C26(H26), C29(H29), C41(H41), 
 C44(H44), C56(H56), C59(H59) 
2.b Secondary CH2 refined with riding coordinates: 
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B) 
2.c Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4A), C5(H5), C22(H22), C23(H23), C24(H24), C37(H37), C38(H38), 
 C39(H39), C54(H54), C53(H53), C52(H52) 
2.d Idealised Me refined as rotating group: 
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C11(H11A,H11B,H11C), C12(H12A,H12B, 
H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C14(H14A,H14B, 
H14C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A, 
H31B,H31C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), 
C45(H4,H45A,H45B), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,H57B, 
H57C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C63(H63A, 
H63B,H63C), C64(H64A,H64B,H64C) 
;