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_4085965
_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         'C64.00 H90 Co1 N3 O2.00 P3 Si1 Zr1'
_chemical_formula_sum            'C64 H90 Co N3 O2 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             11-11-10
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.1775(12)
_cell_length_b                   19.1775(12)
_cell_length_c                   32.006(2)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     10194.0(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.026
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6633
_diffrn_reflns_theta_full        30.025
_diffrn_reflns_theta_max         30.025
_diffrn_reflns_theta_min         1.767
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3821.999
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.470
_exptl_crystal_size_min          0.240
_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 ether in a 
volume of 1554.6 \%A3 per unit cell (15.3%).  It appeared 
that the cavity areas contained about six ether molecules, 
located near the centers of symmetry at (0, 0, 0), 
(0.333, 0.667, 0.667) and (0.667, 0.333, 0.333) as shown  
in the ac projection above.  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 225 e- per unit cell, likely representing six 
ether molecules, consistent with our earlier observations.  
Use of the SQUEEZE technique resulted in a decrease of 
ca. 1.4 % in R. 
;
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.0040076
_refine_ls_shift/su_mean         0.0001282
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +15.09P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0741
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0741
_reflns_limit_h_max              13
_reflns_limit_h_min              -26
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                6228
_reflns_number_total             6633
_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   0.0284
_oxford_refine_ls_scale          0.040230(3)
_oxford_reflns_number_all        6633
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jk_82_0m in R-3'
_cod_data_source_file            om5b00182_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085963--4085969.cif.
;
_cod_original_cell_volume        10194.1(11)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C64.00 H90 Co1 N3 O2.00 P3 Si1 Zr1'
_cod_database_code               4085965
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT ZR   (    1 ,X'S,U'S)  UNTIL SI   (    1 ) 
CONT O    (    1 ,X'S,U[ISO]) 
CONT O    (    2 ,X'S,U'S)  UNTIL N    (    1 ) 
CONT C    (    1 ,X'S,U[ISO]) 
CONT C    (    2 ,X'S,U'S)  UNTIL C    (   22 ) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,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) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;