Multi-electron reduction facilitated by a trianionic pyridine(diimine) ligand
Dennis P. Cladis; John J. Kiernicki; Phillip E. Fanwick; Suzanne C. Bart; Chem.Commun. 49 (2013) 4169–; doi:10.1039/c2cc37193f

data_7109231
_publ_section_title
;
 Multi-electron reduction facilitated by a trianionic pyridine(diimine)
 ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              4169
_journal_paper_doi               10.1039/c2cc37193f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C49 H56 N5 U1,C4 H8 O1,C7 H8'
_chemical_formula_sum            'C60 H72 N5 O U'
_chemical_formula_weight         1117.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9021(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.6610(7)
_cell_length_b                   22.0109(8)
_cell_length_c                   26.2485(7)
_cell_measurement_reflns_used    19956
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      1
_cell_volume                     10780.1(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9460
_diffrn_measured_fraction_theta_max 0.9460
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter
chi circle and a 200 degree curved image plate at a fixed
distance of 127.4mm. Strategy was optimized using the
CrystalClear software. The completeness is the best
that can be obtained with this geometry. The missing data are not cusp
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number
of observed data as inconsistent equivalents are removed
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            112480
_diffrn_reflns_theta_full        70.2
_diffrn_reflns_theta_max         70.24
_diffrn_reflns_theta_min         2.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.802
_exptl_absorpt_correction_T_max  0.4147
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         2.91
_refine_diff_density_min         -1.95
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1234
_refine_ls_number_reflns         19423
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+25.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.174
_refine_ls_wR_factor_ref         0.183
_reflns_number_gt                16093
_reflns_number_total             19423
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c2cc37193f.txt
_cod_data_source_block           2DC96
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'C60 H72 N5 O1 U1'
_cod_database_code               7109231