Construction of zirconium/hafnium-oxo clusters based on a new protection-calix[8]arene.
Wang, Fei-Fei; Hou, Baoshan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6507–6514; doi:10.1039/d4dt00169a

data_7715490
_publ_section_title
;
 Construction of zirconium/hafnium-oxo clusters based on a new
 protection-calix[8]arene.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6507
_journal_page_last               6514
_journal_paper_doi               10.1039/d4dt00169a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C184 H226 Hf8 N2 O35, 8CH3OH, 7C3H7NO'
_chemical_formula_sum            'C213 H307 Hf8 N9 O50'
_chemical_formula_weight         5221.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-03-02 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.524(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.070(4)
_cell_length_b                   30.684(5)
_cell_length_c                   17.217(6)
_cell_measurement_reflns_used    9335
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      63.858
_cell_measurement_theta_min      3.933
_cell_volume                     10671(5)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      290.56
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55861
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        64.436
_diffrn_reflns_theta_max         64.436
_diffrn_reflns_theta_min         2.677
_exptl_absorpt_coefficient_mu    7.415
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.329
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     1229
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.1020
_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^)+(0.1331P)^2^+347.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2682
_refine_ls_wR_factor_ref         0.2960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6868
_reflns_number_total             8967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00169a2.cif
_cod_data_source_block           Hf8
_cod_depositor_comments
'Adding full bibliography for 7715487--7715490.cif.'
_cod_original_cell_volume        10672(5)
_cod_database_code               7715490
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H42B-H43B
 1.8 with sigma of 0.02
 H13-H47A
 1.8 with sigma of 0.02
 H44B-H45B
 1.8 with sigma of 0.02
 C42-C36 = C43-C36 = C46-C36 = C44-C26 = C47-C26 = C45-C26
 1.5 with sigma of 0.02
 O10-O2
 2.47 with sigma of 0.02
 C47-C44 \\sim C45-C44 \\sim C47-C45
 with sigma of 0.02
 C44-C26 \\sim C47-C26 \\sim C45-C26
 with sigma of 0.02
 C35-C27 \\sim C39-C35 \\sim C39-C27
 with sigma of 0.02
 C39-C28 \\sim C35-C28 \\sim C28-C27
 with sigma of 0.02
 C44-C12 \\sim C47-C12 \\sim C45-C12
 with sigma of 0.02
 C40-C38 \\sim C41-C38 \\sim C41-C40
 with sigma of 0.02
 C41-C37 \\sim C40-C37 \\sim C38-C37
 with sigma of 0.02
 C46-C43 \\sim C42-C43 \\sim C42-C46
 with sigma of 0.02
 C42-C36 \\sim C36-C43 \\sim C46-C36
 with sigma of 0.02
 C46-C6 \\sim C43-C6 \\sim C42-C6
 with sigma of 0.02
3. Rigid bond restraints
 Hf1, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
O10: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Hf2(0.8) Hf3(0.3) Hf4(0.2) Hf5(0.2) O8(0.3) O10(0.25) O11(0.2)
 O13(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B)
6.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C13(H13), C18(H18), C20(H20), C31(H31), C33(H33)
6.d Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C9(C10,C11,C12,C13,C14), C16(C17,C18,C19,C20,C21),
 C29(C30,C31,C32,C33,C34)
6.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              38560
_shelx_fab_checksum              23496
_olex2_submission_special_instructions 'No special instructions were received'