Altering the solubility of metal-organic polyhedra <i>via</i> pendant functionalization of Cp<sub>3</sub>Zr<sub>3</sub>O(OH)<sub>3</sub> nodes.
Sullivan, Meghan G.; Sokolow, Gregory E.; Jensen, Eric T.; Crawley, Matthew R.; MacMillan, Samantha N.; Cook, Timothy R.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 338–346; doi:10.1039/d2dt03401h

data_7711922
_publ_section_title
;
 Altering the solubility of metal-organic polyhedra <i>via</i> pendant
 functionalization of Cp<sub>3</sub>Zr<sub>3</sub>O(OH)<sub>3</sub> nodes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              338
_journal_page_last               346
_journal_paper_doi               10.1039/d2dt03401h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C148 H118 F15 O40 Zr12, C159 H129 F15 O40 Zr12, 8(Cl), C3 N O, 46[C3H7NO]'
_chemical_formula_sum            'C310 H247 Cl8 F30 N O81 Zr24'
_chemical_formula_weight         8324.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2022-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.5390(7)
_cell_length_b                   32.1758(3)
_cell_length_c                   105.6671(10)
_cell_measurement_reflns_used    44160
_cell_measurement_temperature    101.6(5)
_cell_measurement_theta_max      51.2350
_cell_measurement_theta_min      2.0710
_cell_volume                     120379(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      101.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.729
_diffrn_measured_fraction_theta_max 0.729
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 184.00   0.25    1.25 -50.60 -53.63   0.00    --   736
  2  \f    184.00 328.00   0.25    1.25   0.00 -53.63  40.00    --   576
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.729
_diffrn_reflns_Laue_measured_fraction_max 0.729
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_limit_l_min       -107
_diffrn_reflns_number            129856
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        51.834
_diffrn_reflns_theta_max         51.834
_diffrn_reflns_theta_min         2.080
_exptl_absorpt_coefficient_mu    4.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             33024
_refine_diff_density_max         2.151
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3265
_refine_ls_number_reflns         48746
_refine_ls_number_restraints     3880
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1890P)^2^+1183.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2973
_refine_ls_wR_factor_ref         0.3179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33492
_reflns_number_total             48746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03401h2.cif
_cod_data_source_block           wit_exp_1837_auto
_cod_depositor_comments
'Adding full bibliography for 7711919--7711923.cif.'
_cod_original_cell_volume        120378(3)
_cod_database_code               7711922
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H015 of O015, H011 of O011, H01E of O01E, H01F of O01F,
  H01P of O01P, H01W of O01W, H01Z of O01Z, H01G of O01G, H01X of O01X, H01Y of
  O01Y, H022 of O022, H01K of O01K, H023 of O023, H025 of O025, H02A of O02A,
  H01Q of O01Q, H028 of O028, H02I of O02I, H02J of O02J, H02C of O02C, H02S of
  O02S, H02O of O02O, H02Q of O02Q, H02U of O02U, All C(H,H) groups
 At 1.5 times of:
  H034 of O034, H02P of O02P
2. Restrained distances
 C14-C097
 1.49 with sigma of 0.02
 C50-C07L
 1.49 with sigma of 0.02
 C25-C0DJ
 1.6 with sigma of 0.02
 O02P-H02P
 0.87 with sigma of 0.01
 O034-H034
 0.87 with sigma of 0.01
 C06D-H034
 1.866797 with sigma of 0.02
 Zr0H-H034
 2.716117 with sigma of 0.02
 Zr0M-H02P
 2.816355 with sigma of 0.02
 C06A-H02P
 1.867112 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Others
 Sof(F0AJ)=Sof(F0B0)=Sof(F0CO)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F72)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Fixed Sof: F09D(0.5) F0BN(0.5) F0C0(0.5) C14(0.5) F1B(0.5) F1C(0.5) F1D(0.5)
 C1Y(0.5) C1Z(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C25(0.5) C26(0.5)
 H26(0.5) C27(0.5) H27(0.5)
6.a Free rotating group:
 F2(F3,F4,C5,C6,C7,C8,C9,C10,C11), F1(F5,F6,C1,C2,C3,C4,C12,C13,C15), F7(F8,F9,
 C16,C17,C18,C19,C1A,C1B,C1C), F10(F11,F12,C1D,C1E,C1F,C1G,C1H,C1I,C1J),
 F15(F16,F17,C1K,C1L,C1M,C1N,C1O,C1P,C1Q), F18(F19,F1A,C1R,C1S,C1T,C1U,C1V,C1W,
 C1X), F1B(F1C,F1D,C1Y,C1Z,C22,C23,C25,C26,C27), F1H(F1I,F1J,C24,C2E,C2F,C2G,
 C2H,C2I,C2J)
6.b Ternary CH refined with riding coordinates:
 C09X(H09X), C0B2(H0B2), C0BF(H0BF), C0BU(H0BU), C0C3(H0C3)
6.c Secondary CH2 refined with riding coordinates:
 C07C(H07A,H07B), C07J(H07C,H07D), C085(H08A,H08B), C09H(H09B,H09C), C0A1(H0AA,
 H0AB), C0A4(H0AD,H0AE), C0BW(H0BA,H0BC), C0C7(H0CA,H0CB), C0CB(H0CE,H0CF),
 C0CD(H0CC,H0CD)
6.d Aromatic/amide H refined with riding coordinates:
 O011(H011), O015(H015), O01E(H01E), O01F(H01F), O01G(H01G), O01K(H01K),
 O01P(H01P), O01Q(H01Q), O01W(H01W), O01X(H01X), O01Y(H01Y), O01Z(H01Z),
 O022(H022), O023(H023), O025(H025), O028(H028), O02A(H02A), O02C(H02C),
 O02I(H02I), O02J(H02J), O02O(H02O), O02Q(H02Q), O02S(H02S), O02U(H02U),
 C039(H039), C03A(H03A), C03B(H03B), C03I(H03I), C03K(H03K), C03N(H03N),
 C03O(H03O), C03Q(H03Q), C03S(H03S), C03T(H03T), C03W(H03W), C03Y(H03Y),
 C041(H041), C046(H046), C04C(H04C), C04H(H04H), C04J(H04J), C04O(H04O),
 C04Q(H04Q), C04U(H04U), C04W(H04W), C04Z(H04Z), C050(H050), C051(H051),
 C052(H052), C055(H055), C05E(H05E), C05F(H05F), C05H(H05H), C05I(H05I),
 C05K(H05K), C05M(H05M), C05Q(H05Q), C05R(H05R), C05T(H05T), C074(H074),
 C05P(H05P), C06Q(H06Q), C072(H072), C05V(H05V), C05Z(H05Z), C061(H061),
 C063(H063), C065(H065), C067(H067), C069(H069), C06B(H06B), C09N(H09N),
 C07N(H07N), C0B1(H0B1), C0AF(H0AF), C06I(H06I), C06K(H06K), C06L(H06L),
 C06N(H06N), C06O(H06O), C06P(H06P), C06S(H06S), C06T(H06T), C06X(H06X),
 C06Y(H06Y), C06Z(H06Z), C071(H071), C073(H073), C075(H075), C076(H076),
 C077(H077), C078(H078), C079(H079), C07B(H07F), C07D(H07I), C07E(H07E),
 C07F(H07J), C07G(H07G), C07H(H07H), C07I(H07K), C07O(H07O), C07P(H07P),
 C07Q(H07Q), C07R(H07R), C07S(H07S), C07T(H07T), C07V(H07V), C07Z(H07Z),
 C080(H080), C081(H081), C086(H086), C08A(H08C), C08B(H08D), C08G(H08G),
 C08H(H08H), C08I(H08I), C08J(H08J), C08L(H08L), C08O(H08O), C08R(H08R),
 C08S(H08S), C08T(H08T), C08V(H08V), C05S(H05S), C0AB(H0AC), C0AK(H0AK),
 C08W(H08W), C08Y(H08Y), C08Z(H08Z), C090(H090), C091(H091), C093(H093),
 C096(H096), C0B9(H0B9), C088(H088), C056(H056), C0AW(H0AW), C09A(H09A),
 C09E(H09E), C09F(H09F), C09G(H09G), C09I(H09I), C09J(H09J), C09K(H09K),
 C09L(H09L), C09M(H09M), C09O(H09O), C09P(H09P), C09Q(H09Q), C09R(H09R),
 C09T(H09T), C09V(H09V), C09Y(H09Y), C09Z(H09Z), C0A0(H0A0), C0A3(H0A3),
 C0A8(H0A8), C0A9(H0A9), C0AE(H0AH), C0AG(H0AG), C0AI(H0AI), C0AL(H0AL),
 C0AO(H0AO), C0AP(H0AP), C0AX(H0AX), C0AZ(H0AZ), C0B4(H0B4), C0B6(H0B6),
 C0B7(H0B7), C0BB(H0BB), C0BD(H0BD), C0BE(H0BE), C0BH(H0BH), C0BI(H0BI),
 C0BJ(H0BJ), C0BL(H0BL), C0BP(H0BP), C0BR(H0BR), C0BX(H0BX), C0B5(H0B5),
 C0AY(H0AY), C0A5(H0A5), C0B8(H0B8), C0C1(H0C1), C276(H276), C57(H57),
 C0DK(H0DK), C196(H196), C0DV(H0DV), C0DY(H0DY), C7(H7), C8(H8), C10(H10),
 C11(H11), C3(H3), C4(H4), C13(H13), C15(H15), C18(H18), C19(H19), C1B(H1B),
 C1C(H1C), C1F(H1F), C1G(H1G), C1I(H1I), C1J(H1J), C1M(H1M), C1N(H1N), C1P(H1P),
  C1Q(H1Q), C1T(H1T), C1U(H1U), C1W(H1W), C1X(H1X), C22(H22), C23(H23),
 C26(H26), C27(H27), C2F(H2F), C2G(H2G), C2I(H2I), C2J(H2J)
6.e Fitted pentagon refined as free rotating group:
 C05T(C074,C05P,C06Q,C072), C06F(C09N,C07N,C0B1,C0AF), C08V(C05S,C0AB,C0AK,
 C05G), C0BX(C0B5,C0AY,C0A5,C0B8)
6.f Fitted hexagon refined as free rotating group:
 C096(C08Q,C0B9,C088,C056,C0AW), C0D6(C276,C57,C097,C0DK,C196)
;
_shelx_res_checksum              76092
_shelx_hkl_checksum              40163
_shelx_fab_checksum              43577
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;