Group 13 ion coordination to pyridyl models NAD+ reduction potentials
Parsons, Leo W.; Fettinger, James C.; Berben, Louise; Chemical Communications  (2023) –; doi:10.1039/D3CC02562D

data_7131778
_publ_section_title
;
 Group 13 ion coordination to pyridyl models NAD+ reduction potentials
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02562D
_journal_year                    2023
_chemical_formula_moiety         'I8 Pb2, 4(C12 H14 N O)'
_chemical_formula_sum            'C48 H56 I8 N4 O4 Pb2'
_chemical_formula_weight         2182.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1zshx5
_audit_creation_date             2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-01 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.668(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5228(17)
_cell_length_b                   12.4668(17)
_cell_length_c                   39.555(6)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.356
_cell_measurement_theta_min      2.912
_cell_volume                     6120.1(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            52790
_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         25.392
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.571
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1295 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.6261. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             3968
_exptl_crystal_preparation
'Prepared from 2:1 solution of cation:lead (II) iodide disolved in GBL with vapor diffusion of DCM.'
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.584
_refine_diff_density_min         -4.336
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Flack x determined using 4603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0133P)^2^+199.3977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10289
_reflns_number_total             10978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02562d2.cif
_cod_data_source_block           1_napthyl_ethyl
_cod_original_cell_volume        6120.0(15)
_cod_database_code               7131778
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.152
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.625(10)
 0.375(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Rigid body (RIGU) restrains
 C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C35(H35A,
 H35B), C36(H36A,H36B), C47(H47A,H47B), C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C45(H45)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_shelx_res_checksum              32371
_shelx_hkl_checksum              52691
_olex2_exptl_crystal_mounting_method
'Mounted on kapton loop at RT using grease to fixcrystal in place.'
_olex2_submission_special_instructions 'No special instructions were received'