Spin-State Crossover with Structural Changes in a Cobalt(II) Organometallic Species: Low-Coordinate, First Row, Heteroleptic Amido Transition Metal Aryls. Synthesis and Characterization of Ar'MN(H)Ar# (M = Mn, Fe, Co) (Ar' = C6H3-2,6-(C6H3-2,6-iPr2)2, Ar#= C6H3-2,6-(C6H2-2,4,6-Me3)2)
Chengbao Ni; James C. Fettinger; Gary J. Long; Philip P. Power; Inorganic Chemistry 48 (2009) 2443–2448; doi:10.1021/ic801660a

data_4301657
_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
;
Spin-State Crossover with Structural Changes in a Cobalt(II) Organometallic
Species: Low-Coordinate, First Row, Heteroleptic Amido Transition Metal
Aryls. Synthesis and Characterization of Ar'MN(H)Ar# (M = Mn, Fe, Co)
(Ar' = C6H3-2,6-(C6H3-2,6-iPr2)2, Ar#= C6H3-2,6-(C6H2-2,4,6-Me3)2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2443
_journal_page_last               2448
_journal_paper_doi               10.1021/ic801660a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C54 H63 Co N'
_chemical_formula_sum            'C54 H63 Co N'
_chemical_formula_weight         784.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.042(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.962(5)
_cell_length_b                   11.288(3)
_cell_length_c                   19.485(5)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.813
_cell_volume                     4277.3(19)
_computing_cell_refinement       'SAINT (7.46A) (Bruker, 2006)'
_computing_data_collection       'Apex2 (2.1-4) (Bruker, 2007)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0310
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_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7731
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.8848
_exptl_absorpt_correction_type   'Empirical, Twinabs (multi-scan)'
_exptl_absorpt_process_details   'TWINABS V2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+12.2232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                6657
_reflns_number_total             7731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801660a_si_001_3.cif
_cod_data_source_block           tw44
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4277.5(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301657