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_7039562
_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         'C67 H104 Co1 N6 O1 P3 Zr1'
_chemical_formula_sum            'C67 H104 Co N6 O P3 Zr'
_chemical_formula_weight         1252.68
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-07
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_audit_update_record
;
2016-06-10 deposited with the CCDC.
2016-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0071(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2422(2)
_cell_length_b                   15.6852(3)
_cell_length_c                   38.6830(9)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    120
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6821.2(2)
_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  0.060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            94527
_diffrn_reflns_theta_full        26.019
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         1.053
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         13414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0011856
_refine_ls_shift/su_mean         0.0000285
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 4.65P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0809
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0809
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              47
_reflns_limit_l_min              0
_reflns_number_gt                10734
_reflns_number_total             13414
_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   0.0417
_oxford_refine_ls_scale          0.065822(6)
_oxford_reflns_number_all        13414
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CTV_13_0m in P2(1)/n'
_cod_data_source_file            c6dt01498d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7039558--7039562.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C67 H104 Co1 N6 O1 P3 Zr1'
_cod_database_code               7039562
_solvent_exptl_crystal_recrystallization_method 'diethyl ether'