Synthesis, Characterization, and Magnetism of Divalent Aryl Transition-Metal Complexes of the Simplest Dialkylamide, NMe2: Rare T-Shaped Coordination at Chromium
Chengbao Ni; Gary J. Long; Fernande Grandjean; Philip P. Power; Inorganic Chemistry 48 (2009) 11594–11600; doi:10.1021/ic901462t

data_4303834
_publ_contact_author_address
;
Department of Chemistry
University of California, Davis
1 Shields Ave
Davis, CA 95616
;
_publ_contact_author_email       pppower@ucdavis.edu
_publ_contact_author_name        'Power, Philip P.'
_publ_section_title
;
Synthesis, Characterization, and Magnetism of Divalent Aryl
Transition-Metal Complexes of the Simplest Dialkylamide, NMe2: Rare
T-Shaped Coordination at Chromium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11594
_journal_page_last               11600
_journal_paper_doi               10.1021/ic901462t
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C67.76 H97.28 Cr3 I0.12 N3.88'
_chemical_formula_weight         1137.44
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2249(11)
_cell_length_b                   16.8147(11)
_cell_length_c                   21.8935(14)
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.394
_cell_measurement_theta_min      2.205
_cell_volume                     6341.0(7)
_computing_cell_refinement       'SAINT (7.46A) (Bruker, 2006)'
_computing_data_collection       'SMART 1000'
_computing_data_reduction        'SAINT (7.46A) (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76561
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/3 (Sheldrick, 2007)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2437
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+6.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                5259
_reflns_number_total             7279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901462t_si_002_1.cif
_cod_data_source_block           cbn31f
_cod_database_code               4303834