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_4085966
_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         'C76 H101 Co1 N5 O1 P3 Si1 Zr1'
_chemical_formula_sum            'C76 H101 Co N5 O P3 Si Zr'
_chemical_formula_weight         1371.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-18
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                67.337(6)
_cell_angle_beta                 77.173(6)
_cell_angle_gamma                79.696(6)
_cell_formula_units_Z            2
_cell_length_a                   15.4086(12)
_cell_length_b                   15.4255(13)
_cell_length_c                   17.9455(15)
_cell_measurement_reflns_used    3757
_cell_measurement_temperature    135
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     3817.1(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      135
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.108
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14887
_diffrn_reflns_theta_full        25.480
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.247
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.070
_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 473 \%A3 per unit cell (12.4%).  It appeared 
that the cavity areas contained about two pentane 
molecules, located near a center of symmetry at 
(0, 0.500, 0.500). 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 SQUEEZE6,7 technique, in order to produce 
a ?solvate-free? structure factor set.  PLATON reported 
a total electron density of 107 e- per unit cell in large 
voids, likely representing about two-to-three pentane molecules, 
consistent with our earlier observations.  Use of 
the SQUEEZE technique resulted in a decrease of 
ca. 2.0 % in R.
;
_refine_diff_density_max         1.25
_refine_diff_density_min         -1.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0005959
_refine_ls_shift/su_mean         0.0000175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.19P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1095
_reflns_limit_h_max              19
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                9196
_reflns_number_total             14887
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.38
_oxford_diffrn_Wilson_scale      105.42
_oxford_refine_ls_r_factor_ref   0.1060
_oxford_refine_ls_scale          0.104085(18)
_oxford_reflns_number_all        14887
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'JK_508_0m in P-1'
_cod_data_source_file            om5b00182_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4085963--4085969.cif.'
_cod_original_cell_volume        3817.1(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C76 H101 Co1 N5 O1 P3 Si1 Zr1'
_cod_database_code               4085966