Multi-electron redox processes at a Zr(iv) center facilitated by an appended redox-active cobalt-containing metalloligand.
Krogman, Jeremy P.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11182–11190; doi:10.1039/c6dt01498d

data_7039558
_publ_section_title
;
 Multi-electron redox processes at a Zr(iv) center facilitated by an
 appended redox-active cobalt-containing metalloligand.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11182
_journal_page_last               11190
_journal_paper_doi               10.1039/c6dt01498d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C63 H103 Co1 N5 O1 P3 Zr1'
_chemical_formula_sum            'C63 H103 Co N5 O P3 Zr'
_chemical_formula_weight         1189.62
_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     other
_audit_creation_date             2014-10-23
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                89.6031(17)
_cell_angle_beta                 74.4605(15)
_cell_angle_gamma                75.7836(15)
_cell_formula_units_Z            2
_cell_length_a                   12.6423(4)
_cell_length_b                   12.9539(4)
_cell_length_c                   21.9518(7)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     3350.82(19)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_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  0.067
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14495
_diffrn_reflns_theta_full        25.157
_diffrn_reflns_theta_max         27.051
_diffrn_reflns_theta_min         1.930
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272.000
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
During the structure solution, electron density difference maps 
revealed that there were likely two molecules of solvent in the 
asymmetric unit. From history, the remaining solvate was likely 
tetrahydrofuran(THF). One of the molecules of THF was in a volume 
of 314 \%A3 per unit cell (9.4%).  It appeared that the cavity 
areas contained about two THF molecules, located near the center 
of symmetry at (0.500, 0.500, 0) as shown in the ac projection 
below.  Modeling this THF molecule 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.  
PLATON reported a total electron density of 62 e- per unit cell, 
likely representing about two THF molecules, consistent with our 
earlier observations.  Use of the SQUEEZE technique resulted 
in a decrease of ca. 3.8 % in R.   
;
_refine_diff_density_max         1.46
_refine_diff_density_min         -1.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9534
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         14495
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.0104006
_refine_ls_shift/su_mean         0.0001970
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 2.90P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1307
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1307
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                10838
_reflns_number_total             14495
_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   0.0713
_oxford_refine_ls_scale          0.11383(3)
_oxford_reflns_number_all        14495
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'JK_742_0m in P-1'
_cod_data_source_file            c6dt01498d2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039558--7039562.cif.
;
_cod_original_cell_volume        3350.82(11)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C63 H103 Co1 N5 O1 P3 Zr1'
_cod_database_code               7039558