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_7717045
_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 Zr, H12 Fe O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Fe Mo6 N18 O48 Zr'
_chemical_formula_weight         2490.76
_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
_cell_length_a                   21.8319(4)
_cell_length_b                   21.8319(4)
_cell_length_c                   14.7616(3)
_cell_measurement_reflns_used    8062
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      29.7740
_cell_measurement_theta_min      2.9210
_cell_volume                     6093.2(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      102(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10009
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.558
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95349
_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            'pale yellow'
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       plate
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 2217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5470
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0387P)^2^+24.1811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.802
_reflns_Friedel_fraction_max     0.757
_reflns_number_gt                5319
_reflns_number_total             5470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02120g2.cif
_cod_data_source_block           FeZrMo6
_cod_depositor_comments
'Adding full bibliography for 7717042--7717049.cif.'
_cod_original_cell_volume        6093.2(3)
_cod_database_code               7717045
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              95360
_shelx_hkl_checksum              55131