Formation and Subsequent Reactivity of a N2-Stabilized Cobalt–Hydride Complex
Krogman, Jeremy P.; Foxman, Bruce M.; Thomas, Christine M.; Organometallics 34 (2015) 3159–; doi:10.1021/acs.organomet.5b00182

data_4085964
_publ_section_title
;
 Formation and Subsequent Reactivity of a N2-Stabilized Cobalt--Hydride
 Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3159
_journal_paper_doi               10.1021/acs.organomet.5b00182
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C63 H90 Co1 N5 O1 P3 Si1 Zr1'
_chemical_formula_sum            'C63 H90 Co N5 O P3 Si Zr'
_chemical_formula_weight         1204.60
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-02-17
_audit_creation_method           CRYSTALS_ver_14.41
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.2253(7)
_cell_length_b                   19.2253(7)
_cell_length_c                   31.9514(11)
_cell_measurement_reflns_used    9038
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     10227.4(6)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6676
_diffrn_reflns_theta_full        29.538
_diffrn_reflns_theta_max         30.141
_diffrn_reflns_theta_min         1.379
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3822.000
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.310
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there were considerable disordered solvent 
molecules, which could not be successfully modeled.  From 
history, the remaining solvate was likely pentane in a volume 
of 1680.7 \%A3 per unit cell (16.4%).  It appeared that the 
cavity areas contained about nine pentane molecules, 
located on near the  the rotary inversion axes -3 axes 
at (0, 0, 0.500), (0.333, 0.667, 0.167) and (0.667, 0.333, 0.833). 
Modeling with or without restraints was unsuccessful, as was 
step by step acquisition of peaks using successive electron 
density difference maps. Thus, the structure factors were 
modified using the PLATON SQUEEZE technique, in order to 
produce a ?solvate-free?  structure factor set.  PLATON 
reported a total electron density of 320 e- per unit cell, 
likely representing about nine pentane molecules, consistent 
with our earlier observations.  Use of the SQUEEZE technique 
resulted in a decrease of ca. 3.2 % in R.  
;
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.0037362
_refine_ls_shift/su_mean         0.0001021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +29.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0896
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0896
_reflns_limit_h_max              13
_reflns_limit_h_min              -27
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                5923
_reflns_number_total             6676
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0361
_oxford_refine_ls_scale          0.049150(6)
_oxford_reflns_number_all        6676
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'JK_754_0m in R-3'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            om5b00182_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085963--4085969.cif.'
_cod_original_sg_symbol_Hall     -R3
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C63 H90 Co1 N5 O1 P3 Si1 Zr1'
_cod_database_code               4085964