A proton-responsive ligand becomes a dimetal linker for multisubstrate assembly <i>via</i> nitrate deoxygenation.
Cabelof, Alyssa C.; Carta, Veronica; Caulton, Kenneth G.; Chemical communications (Cambridge, England) 57 (2021) 2780–2783; doi:10.1039/d0cc07886g

data_7127916
_publ_section_title
;
 A proton-responsive ligand becomes a dimetal linker for multisubstrate
 assembly <i>via</i> nitrate deoxygenation.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2780
_journal_page_last               2783
_journal_paper_doi               10.1039/d0cc07886g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C30 H26 N7 Ni O3, N O3'
_chemical_formula_sum            'C30 H26 N8 Ni O6'
_chemical_formula_weight         653.30
_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
_atom_sites_solution_primary     dual
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2020-11-02 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_measurement_temperature    173
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      3.03
_cell_volume                     2941.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.994
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17798
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         2.435
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex3 (Bruker,2016)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.261
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0514
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.2258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4034
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7127916--7127921.cif.'
_cod_database_code               7127916
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_shelx_estimated_absorpt_t_max   0.932
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_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.a Aromatic/amide H refined with riding coordinates:
 N10(H10), N30(H30), C32(H32), C12(H12), C38(H38), C26(H26), C34(H34), C6(H6),
 C37(H37), C25(H25), C24(H24), C5(H5), C4(H4), C18(H18), C36(H36), C35(H35),
 C14(H14), C15(H15), C17(H17), C16(H16)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              16224
_shelx_hkl_checksum              3056
_olex2_date_sample_data_collection 2019-06-12
_olex2_date_sample_submission    2019-06-11
_olex2_submission_original_sample_id AC2.001
_olex2_submission_special_instructions 'No special instructions were received'