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_7127920
_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         'C34 H30 Br2 N8 Ni2'
_chemical_formula_sum            'C34 H30 Br2 N8 Ni2'
_chemical_formula_weight         827.90
_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
_atom_sites_solution_primary     dual
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;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.5070(10)
_cell_angle_beta                 106.9510(10)
_cell_angle_gamma                100.1250(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0659(3)
_cell_length_b                   9.0221(3)
_cell_length_c                   12.1370(5)
_cell_measurement_reflns_used    5507
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.69
_cell_volume                     830.00(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
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_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      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0804
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28559
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.571
_diffrn_reflns_theta_min         2.298
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.579
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method 'from a concentrated CD3CN solution'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3967
_reflns_number_total             5104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07886g2.cif
_cod_data_source_block           mo_20041_0m
_cod_depositor_comments
'Adding full bibliography for 7127916--7127921.cif.'
_cod_database_code               7127920
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C11(H11), C5(H5), C12(H12), C15(H15), C14(H14), C13(H13),
 C4(H4)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              88366
_shelx_hkl_checksum              32270
_olex2_date_sample_data_collection 2020-03-12
_olex2_date_sample_submission    2020-03-12
_olex2_submission_original_sample_id 'NMR tube--AC2.190'
_olex2_submission_special_instructions 'No special instructions were received'