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_7704500
_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 H31 Co N6 O6 P, C H2 Cl2'
_chemical_formula_sum            'C24 H33 Cl2 Co N6 O6 P'
_chemical_formula_weight         662.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-15
_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                 90.797(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.203(4)
_cell_length_b                   13.355(4)
_cell_length_c                   12.931(3)
_cell_measurement_reflns_used    1679
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      19
_cell_measurement_theta_min      3
_cell_volume                     2970.6(13)
_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 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17205
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.072
_diffrn_reflns_theta_max         25.072
_diffrn_reflns_theta_min         1.931
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       plate
_exptl_crystal_F_000             1372
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method
'vapor diffusion of cyclohexane in dichloromethane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4789
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1925
_refine_ls_R_factor_gt           0.1040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1509P)^2^+11.9261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2580
_refine_ls_wR_factor_ref         0.3087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2469
_reflns_number_total             4789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01298j2.cif
_cod_data_source_block           mo_17129_0ma
_cod_depositor_comments
'Adding full bibliography for 7704499--7704501.cif.'
_cod_original_cell_volume        2970.5(13)
_cod_database_code               7704500
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-Cl2 \\sim C24-Cl12
 with sigma of 0.02
 C24-Cl1 \\sim C24-Cl11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl11) = Uanis(Cl1) = Uanis(Cl12) = Uanis(Cl2)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H24C)=Sof(H24D)=Sof(Cl12)=Sof(Cl11)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(Cl2)=Sof(Cl1)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1(H1A,H1B), C24(H24A,H24B), C24(H24C,H24D)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C3(H3A), C5(H5), C15(H15), C11(H11), C12(H12), C13(H13),
 C14(H14)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              73872
_olex2_submission_special_instructions 'No special instructions were received'