Controlling the symmetry of hexamonodentate 3d-transition metal complexes through symmetry propagation from high-symmetry Ti-Mo and Zr-Mo clusters <i>via</i> hydrogen-bonding interactions.
Mitsuhashi, Ryoji; Imai, Yuya; Sugiarto, ?; Sakiyama, Hiroshi; Kikukawa, Yuji; Hayashi, Yoshihito; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16186–16194; doi:10.1039/d4dt02120g

data_7717044
_publ_section_title
;
 Controlling the symmetry of hexamonodentate 3d-transition metal complexes
 through symmetry propagation from high-symmetry Ti-Mo and Zr-Mo clusters
 <i>via</i> hydrogen-bonding interactions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16186
_journal_page_last               16194
_journal_paper_doi               10.1039/d4dt02120g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Ti, H12 Ni O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Mo6 N18 Ni O48 Ti'
_chemical_formula_weight         2450.30
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_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
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_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
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_diffrn_ambient_temperature      100(2)
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_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0427
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_diffrn_reflns_point_group_measured_fraction_full 0.725
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.120
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_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0980P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.401
_reflns_Friedel_fraction_full    0.452
_reflns_Friedel_fraction_max     0.400
_reflns_number_gt                3976
_reflns_number_total             4240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02120g2.cif
_cod_data_source_block           NiTiMo6_3p23_100K_a
_cod_depositor_comments
'Adding full bibliography for 7717042--7717049.cif.'
_cod_original_cell_volume        5944.3(5)
_cod_database_code               7717044
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              88517
_shelx_hkl_checksum              43358