Chemical tuning of spin clock transitions in molecular monomers based on nuclear spin-free Ni(ii)
Rubín-Osanz, Marcos; Lambert, François; Shao, Feng; Rivière, Eric; Guillot, Régis; Suaud, Nicolas; Guihéry, Nathalie; Zueco, David; Barra, Anne-Laure; Mallah, Talal; Luis, Fernando; Chemical Science 12 (2021) 5123–5133; doi:10.1039/D0SC05856D

data_1560717
_publ_section_title
;
 Chemical tuning of spin clock transitions in molecular monomers based on
 nuclear spin-free Ni(ii)
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              5123
_journal_page_last               5133
_journal_paper_doi               10.1039/D0SC05856D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C16 H27 N8 Ni S, C N S, 0.5(C H4 O)'
_chemical_formula_sum            'C17.5 H29 N9 Ni O0.5 S2'
_chemical_formula_weight         496.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-22 deposited with the CCDC.	2021-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8018(4)
_cell_length_b                   16.4349(4)
_cell_length_c                   19.1348(5)
_cell_measurement_reflns_used    9271
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.76
_cell_measurement_theta_min      2.51
_cell_volume                     4544.6(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            145386
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.858
_diffrn_reflns_theta_min         1.584
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.8465
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.943
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         16791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+4.9647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14103
_reflns_number_total             16791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05856d2.cif
_cod_data_source_block           Ni(imdipa)NCS2
_cod_depositor_comments
;
          Adding full bibliography for 1560717.cif.

2022-04-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     '2(C16 H27 N8 Ni S), 2(C N S), C H4 O '
_cod_original_formula_sum        'C35 H58 N18 Ni2 O S4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     992.65
_cod_database_code               1560717
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.839
_shelx_res_checksum              76638
_shelx_hkl_checksum              68878