Nitrogen oxyanion reduction by Co(ii) augmented by a proton responsive ligand: recruiting multiple metals.
Cabelof, Alyssa C.; Carta, Veronica; Chen, Chun-Hsing; Caulton, Kenneth G.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7891–7896; doi:10.1039/d0dt01298j

data_7704499
_publ_section_title
;
 Nitrogen oxyanion reduction by Co(ii) augmented by a proton responsive
 ligand: recruiting multiple metals.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7891
_journal_page_last               7896
_journal_paper_doi               10.1039/d0dt01298j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C23 H29 Co N5 O3 P, 0.25(C2 H3 N)'
_chemical_formula_sum            'C23.5 H29.75 Co N5.25 O3 P'
_chemical_formula_weight         523.67
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.002(4)
_cell_length_b                   17.002(4)
_cell_length_c                   17.320(4)
_cell_measurement_reflns_used    1460
_cell_measurement_temperature    173
_cell_measurement_theta_max      19.34
_cell_measurement_theta_min      2.35
_cell_volume                     5007(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15185
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.065
_diffrn_reflns_theta_max         25.065
_diffrn_reflns_theta_min         1.678
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex3 (Bruker, 2016)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             2188
_exptl_crystal_preparation       Synthesized
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+2.8174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2753
_reflns_number_total             4437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01298j2.cif
_cod_data_source_block           19074
_cod_depositor_comments
'Adding full bibliography for 7704499--7704501.cif.'
_cod_original_cell_volume        5006(3)
_cod_original_formula_sum        'C23.50 H29.75 Co N5.25 O3 P'
_cod_database_code               7704499
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.84(6)
 0.16(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C6A, C6B}
{C2A, C2B}
4. Restrained distances
 N1S-C2S
 1.13 with sigma of 0.02
 N1S-C3S
 2.58 with sigma of 0.02
 Co1A-P1 \\sim Co1B-P1
 with sigma of 0.02
 Co1A-N1A \\sim Co1B-N1B
 with sigma of 0.02
 Co1A-N4A \\sim Co1B-N4B
 with sigma of 0.02
 Co1A-N5A \\sim Co1B-N5B
 with sigma of 0.02
5. Restrained planarity
 C6B, N1B, C2B, C3B, C4B, C5B
 with sigma of 0.1
6. Rigid bond restraints
 N1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1B, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Uiso/Uaniso restraints and constraints
N4A \\sim O1A \\sim O2A \\sim N4B \\sim O1B \\sim O2B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Co1A) = Uanis(Co1B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B)
Uanis(N4A) = Uanis(N4B)
Uanis(N5A) = Uanis(N5B)
Uanis(N1A) = Uanis(N1B)
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
Uanis(C21A) = Uanis(C21B)
Uanis(C22A) = Uanis(C22B)
Uanis(C23A) = Uanis(C23B)
Uiso(N1S) = Uiso(C2S)
Uiso(N1S) = Uiso(C2S) = Uiso(C3S)
8. Same fragment restrains
{N4A, O1A, O2A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N4B, O1B, O2B}
{C20A, C21A, C22A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
{C16A, C17A, C19A, C18A} sigma for 1-2: 0.02, 1-3: 0.04
{C16A, C18A, C17A, C19A} sigma for 1-2: 0.02, 1-3: 0.04
{C16A, C18A, C19A, C17A} sigma for 1-2: 0.02, 1-3: 0.04
{C16A, C19A, C17A, C18A} sigma for 1-2: 0.02, 1-3: 0.04
{C16A, C19A, C18A, C17A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C16A, C17A, C18A, C19A}
{C16A, C17A, C18A, C19A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C21A, C23A, C22A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C22A, C21A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C22A, C23A, C21A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C23A, C21A, C22A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C23A, C22A, C21A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C20A, C21A, C22A, C23A}
{C16A, C17A, C18A, C19A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C21A, C22A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C16B, C17B, C18B, C19B}
{C16A, C17A, C18A, C19A} sigma for 1-2: 0.02, 1-3: 0.04
{C20A, C21A, C22A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C20B, C21B, C22B, C23B}
9. Others
 Sof(Co1B)=Sof(N4B)=Sof(O1B)=Sof(O2B)=Sof(N5B)=Sof(O3B)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(N1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=
 Sof(H5B)=Sof(C6B)=Sof(C16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20B)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(Co1A)=Sof(N4A)=Sof(O1A)=Sof(O2A)=Sof(N5A)=Sof(O3A)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(N1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Fixed Sof: N1S(0.25) C2S(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25) H3SC(0.25)
10.a Riding coordinates:
 C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C17B(H17D,
 H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C21B(H21D,H21E,H21F),
 C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F), C3S(H3SA,H3SB,H3SC)
10.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB)
10.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C3B(H3B), C4B(H4B), C5B(H5B), C8(H8), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15)
10.d Fitted hexagon refined as free rotating group:
 N1A(C2A,C3A,C4A,C5A,C6A), N1B(C2B,C3B,C4B,C5B,C6B)
10.e Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C)
;
_shelx_res_checksum              81633
_olex2_submission_special_instructions 'No special instructions were received'