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_7717042
_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 Fe Mo6 N18 O18 Ti, H12 O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Fe Mo6 N18 O48 Ti'
_chemical_formula_weight         2447.44
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
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_cell_length_b                   21.6648(4)
_cell_length_c                   14.6787(3)
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_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      30.1460
_cell_measurement_theta_min      2.9640
_cell_volume                     5966.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10783
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.577
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17458
_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    2.043
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3690
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4493
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0814P)^2^+42.1115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.478
_reflns_Friedel_fraction_full    0.534
_reflns_Friedel_fraction_max     0.476
_reflns_number_gt                4392
_reflns_number_total             4493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02120g2.cif
_cod_data_source_block           FeTiMo6_3p22_104K_a
_cod_depositor_comments
'Adding full bibliography for 7717042--7717049.cif.'
_cod_original_cell_volume        5966.6(3)
_cod_database_code               7717042
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              78467
_shelx_hkl_checksum              12964