Oxygen activation at a dicobalt centre of a dipyridylethane naphthyridine complex.
Brodsky, Casey N.; Passard, Guillaume; Ullman, Andrew M.; Jaramillo, David E.; Bloch, Eric D.; Huynh, Michael; Gygi, David; Costentin, Cyrille; Nocera, Daniel G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11903–11908; doi:10.1039/c8dt01598h

data_7046641
_publ_section_title
;
 Oxygen activation at a dicobalt centre of a dipyridylethane naphthyridine
 complex.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11903
_journal_page_last               11908
_journal_paper_doi               10.1039/c8dt01598h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C34 H31 Co2 N7 O2, 4(F3 P0.5), C2 H3 N'
_chemical_formula_sum            'C36 H34 Co2 F12 N8 O2 P2'
_chemical_formula_weight         1018.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-04-21 deposited with the CCDC.
2018-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                65.672(4)
_cell_angle_beta                 66.433(4)
_cell_angle_gamma                87.830(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9276(17)
_cell_length_b                   14.7062(19)
_cell_length_c                   14.9906(19)
_cell_measurement_reflns_used    4427
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.500
_cell_measurement_theta_min      2.49
_cell_volume                     2352.7(5)
_computing_cell_refinement       'SAINT 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 v2014.3.0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX II CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2455
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9726
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          .05
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .01
_platon_squeeze_details
;
The unit cell contains 3 disordered diethylether molecules, which have 
been treated as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.

The Platon Squeeze procedure was applied to recover 137 electrons
per unit cell in one void (total volume 559 ^A^3). Disordered solvent
lattice diethylether molecules (42 electrons per Et2O) were present
prior to the application of Squeeze, however, a satisfactory
point atom model could not be achieved. The application of Squeeze gave
a good improvement in the data statistics and allowed for a
full anisotropic refinement of the structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9726
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1872
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                4427
_reflns_number_total             9726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01598h2.cif
_cod_data_source_block           cb_a_with3ethers-sr
_cod_depositor_comments
'Adding full bibliography for 7046640--7046641.cif.'
_cod_database_code               7046641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F6 \\sim P1A-F6A
 with sigma of 0.02
 P1A-F3A \\sim P1-F3
 with sigma of 0.02
 P1A-F2A \\sim P1-F2
 with sigma of 0.02
 P1A-F5A \\sim P1-F5
 with sigma of 0.02
 P1A-F4A \\sim P1-F4
 with sigma of 0.02
 P1-F1 \\sim P1A-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(P1) = Uanis(P1A)
Uanis(F3) = Uanis(F3A)
Uanis(F5) = Uanis(F5A)
Uanis(F4) = Uanis(F4A)
Uanis(F1) = Uanis(F1A)
Uanis(F6) = Uanis(F6A)
Uanis(F2) = Uanis(F2A)
4. Others
 Sof(P1A)=Sof(F3A)=Sof(F5A)=Sof(F4A)=Sof(F1A)=Sof(F6A)=Sof(F2A)=1-FVAR(1)
 Sof(P1)=Sof(F2)=Sof(F1)=Sof(F6)=Sof(F4)=Sof(F3)=Sof(F5)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C00Q(H00Q), C00X(H00X), C00Y(H00Y), C011(H011), C012(H012),
 C013(H013), C015(H015), C016(H016), C017(H017), C01A(H01A), C01C(H01E),
 C01D(H01F), C01F(H01G), C01G(H01H), C01H(H01I), C01I(H01J), C01J(H01K),
 C01M(H01R), C01N(H01S), C01P(H01T)
5.b Idealised Me refined as rotating group:
 C01B(H01B,H01C,H01D), C01K(H01L,H01M,H01N), C01L(H01O,H01P,H01Q), C30(H30A,
 H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'