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_7715487
_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         'C182 H226 O24 Zr4, Cl2, 2CH3OH, 3C3H7NO'
_chemical_formula_sum            'C193 H255 Cl2 N3 O29 Zr4'
_chemical_formula_weight         3516.89
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-03-01 deposited with the CCDC.	2024-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.050(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.4909(13)
_cell_length_b                   22.8712(12)
_cell_length_c                   19.5689(9)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    296.61
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     10049.3(9)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.61
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35632
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        66.848
_diffrn_reflns_theta_max         66.848
_diffrn_reflns_theta_min         2.664
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     2041
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.0928
_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^)+(0.0671P)^2^+136.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5853
_reflns_number_total             8967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00169a2.cif
_cod_data_source_block           Zr4
_cod_depositor_comments
'Adding full bibliography for 7715487--7715490.cif.'
_cod_original_formula_sum        'C193 H255 Cl2 O29 Zr4 N3'
_cod_database_code               7715487
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.604
_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, All O(H) groups
2. Restrained distances
 C55-C33
 1.5 with sigma of 0.02
3. 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 C58 \\sim C46 \\sim C54 \\sim C51
\\sim C53 \\sim C55 \\sim C52 \\sim C47 \\sim C56 \\sim C57 \\sim C48 \\sim C49
\\sim C50: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C53)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O1, Zr1, C1, O1, O3, C14, C17, C1, C4, C11, C30, C9, C29, C14, C17, C3, C3,
 C31, C5, C11, C30, C9, C29, C15, C15, C36, C2, C19, C31, C5, C32, C38, C40,
 C41, O8, C8, C16, C36, C2, C19, C37, C13, C21, C35, C38, C40, C41, O8, C8, C16,
  C47, C47, C10, C42, C45, C58, C46, C54, C52, C13, C21, C35, C7, C25, C10, C42,
  C45, C58, C46, C54, C52, O4, C6, C28, C7, C25, Zr2, C23, C24, C33, O4, C6,
 C28, O6, O2, O2, O5, C18, C39, C43, C44, C51, C53, C55, C23, C24, C33, C12,
 C27, C27, C22, C26, C18, C39, C43, C44, C51, C53, C55, O7, C20, C26, C34, C48,
 C47, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C39(0.7) H39A(0.7) H39B(0.7) H39C(0.7) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C43(0.7) H43A(0.7) H43B(0.7) H43C(0.7) C44(0.7) H44A(0.7)
 H44B(0.7) H44C(0.7) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) H58C(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) H54C(0.5) C51(0.3) H51A(0.3) H51B(0.3) H51C(0.3) C53(0.3) H53A(0.3)
 H53B(0.3) H53C(0.3) C55(0.3) H55A(0.3) H55B(0.3) H55C(0.3) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) H50C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C21(H21A,H21B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26),
 C29(H29), C30(H30)
6.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C46(H46A,H46B,H46C),
 C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C52(H52A,H52B,H52C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
6.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              50316
_shelx_fab_checksum              36081
_olex2_submission_special_instructions 'No special instructions were received'