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_7127917
_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         'C15 H13 Br2 N3 Ni, C4 H8 O'
_chemical_formula_sum            'C19 H21 Br2 N3 Ni O'
_chemical_formula_weight         525.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
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Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
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_audit_update_record
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2020-11-16 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                95.137(2)
_cell_angle_beta                 95.800(2)
_cell_angle_gamma                107.670(2)
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_cell_length_a                   9.3273(4)
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_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker VENTURE D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
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_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
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_diffrn_source_current           1.4
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_diffrn_source_voltage           50.0
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_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2) .'
_exptl_crystal_colour            pink
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_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
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_exptl_crystal_recrystallization_method
'vapor diffusion of pentane into a THF solution'
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_refine_diff_density_max         1.165
_refine_diff_density_min         -0.800
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0327
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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^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3957
_reflns_number_total             4498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07886g2.cif
_cod_data_source_block           mo_20123_0m_a
_cod_depositor_comments
'Adding full bibliography for 7127916--7127921.cif.'
_cod_database_code               7127917
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.823
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_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C16(H16A,H16B), C18(H18A,H18B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C8(H8), C11(H11), C3(H3A), C5(H5), C15(H15), C4(H4), C14(H14),
 C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              23232
_shelx_hkl_checksum              79899
_olex2_submission_special_instructions 'No special instructions were received'