Coordination-Driven Self-Assembly of M10L8 Metal-Organic Bi-capped Square Antiprisms with Adaptable Cavity
Wang, Xue-Zhi; Sun, Meng-Ying; Zheng, Ji; Luo, Dong; Li, Qi; Zhou, Xiao-Ping; Li, Dan; Dalton Transactions  (2019) –; doi:10.1039/C9DT04368C

data_7701969
_publ_section_title
;
 Coordination-Driven Self-Assembly of M10L8 Metal-Organic Bi-capped Square
 Antiprisms with Adaptable Cavity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04368C
_journal_year                    2019
_chemical_formula_moiety
'C88 H98 Cu10 N48 O, 3(Cl O4), Cl0.7 O2, Cl0.3 O2, 6(C3 H7 N O)'
_chemical_formula_sum            'C106 H140 Cl4 Cu10 N54 O23'
_chemical_formula_weight         3315.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc20ncbd
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-06 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.7950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.28850(10)
_cell_length_b                   25.78600(10)
_cell_length_c                   26.57420(10)
_cell_measurement_reflns_used    52455
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4000
_cell_measurement_theta_min      3.3900
_cell_volume                     14278.09(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  27.00   0.50    0.50    --   -0.90 -82.00-150.00   52
  2  \w      9.00  35.00   0.50    0.50    --   -0.90  82.00-120.00   52
  3  \w    -22.00  90.00   0.50    0.50    --    0.90  38.00  60.00  224
  4  \w    -32.00  16.00   0.50    0.50    --    0.90  82.00 -30.00   96
  5  \w     16.00 132.00   0.50    0.50    --  105.10 -82.00 -90.00  232
  6  \w     80.00 171.00   0.50    0.50    --  105.10  57.00  90.00  182
  7  \w     31.00 132.00   0.50    0.50    --  105.10 -57.00 -30.00  202
  8  \w     88.00 128.00   0.50    0.50    --  105.10  82.00  90.00   80
  9  \w    160.00 187.00   0.50    0.50    --  105.10  82.00  60.00   54
 10  \w     88.00 115.00   0.50    0.50    --  105.10 -82.00   0.00   54
 11  \w     73.00 190.00   0.50    0.50    --  105.10  19.00  30.00  234
 12  \w     55.00 139.00   0.50    0.50    --  105.10 -82.00 -20.73  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0222322000
_diffrn_orient_matrix_UB_12      -0.0554943000
_diffrn_orient_matrix_UB_13      -0.0058819000
_diffrn_orient_matrix_UB_21      -0.0566149000
_diffrn_orient_matrix_UB_22      -0.0221139000
_diffrn_orient_matrix_UB_23      0.0136394000
_diffrn_orient_matrix_UB_31      -0.0419914000
_diffrn_orient_matrix_UB_32      0.0003632000
_diffrn_orient_matrix_UB_33      -0.0602236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            83018
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.732
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.991
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         29158
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0992P)^2^+49.0330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26404
_reflns_number_total             29158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04368c2.cif
_cod_data_source_block           cage1
_cod_original_cell_volume        14278.08(13)
_cod_database_code               7701969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONCuCl
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.589
_reflns_odcompleteness_completeness 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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,H) groups
2. Restrained distances
 O4-Cl0A
 1.44 with sigma of 0.01
 O5-Cl0A
 1.44 with sigma of 0.01
 O3-Cl0A
 1.44 with sigma of 0.01
 Cl0A-O2
 1.44 with sigma of 0.01
 Cl2-O27
 1.44 with sigma of 0.01
 Cl2-O25
 1.44 with sigma of 0.01
 Cl2-O24
 1.44 with sigma of 0.01
 Cl2-O26
 1.44 with sigma of 0.01
 Cl0A-O3
 1.44 with sigma of 0.01
 Cl0A-O4
 1.44 with sigma of 0.01
 O5-O3
 2.35 with sigma of 0.02
 O5-O2
 2.35 with sigma of 0.02
 O2-O3
 2.35 with sigma of 0.02
 O5-O4
 2.35 with sigma of 0.02
 O4-O3
 2.35 with sigma of 0.02
 O4-O2
 2.35 with sigma of 0.02
 O26-O25
 2.35 with sigma of 0.02
 O26-O24
 2.35 with sigma of 0.02
 O24-O25
 2.35 with sigma of 0.02
 O26-O27
 2.35 with sigma of 0.02
 O27-O25
 2.35 with sigma of 0.02
 O27-O24
 2.35 with sigma of 0.02
 O25-O24
 2.35 with sigma of 0.02
3. Rigid bond restraints
 O8, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O26, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O26, O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O26, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O24, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O8 \\sim O6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O9 \\sim O6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C12 \\sim O20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O6 \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O6 \\sim O8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O6 \\sim O9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O3 \\sim O26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O24: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O25 \\sim Cl2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C12) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O6) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O20) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O24) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O25) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O26) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O24) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(O25) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(O26) = Uanis(O4)
Uanis(O26) = Uanis(O5)
5. Others
 Fixed Sof: Cl2(0.7) O2(0.75) O26(0.5) Cl0A(0.3) O25(0.5) O24(0.5) O3(0.7)
 O27(0.5) O4(0.25) O5(0.3)
6.a Rotating group:
 O1(H1A,H1B)
6.b Secondary CH2 refined with riding coordinates:
 C037(H03A,H03B), C03D(H03E,H03F), C03G(H03I,H03J), C03H(H03K,H03L), C03K(H03N,
 H03O), C03L(H03P,H03Q), C03M(H03R,H03S), C03O(H03U,H03V), C03P(H03W,H03X),
 C03S(H03,H), C03X(H2AA,HA), C03Y(H3AA,HB), C045(H04A,H04B), C049(H04C,H04D),
 C04C(H04F,H04G), C04F(H04H,H04I), C04L(H04L,H04M), C04M(H04N,H04O), C04Q(H04P,
 H04Q), C04R(H04R,H04S), C04W(H04T,H04U), C04X(H04W,H04X), C050(H05A,H05B),
 C053(H05C,H05D)
6.c Aromatic/amide H refined with riding coordinates:
 C01W(H01W), C020(H020), C023(H023), C024(H024), C026(H026), C028(H028),
 C029(H029), C02A(H02A), C02C(H02C), C02D(H02D), C02G(H02G), C02H(H02H),
 C02I(H02I), C02J(H02J), C02K(H02K), C02N(H02N), C02P(H02P), C02Q(H02Q),
 C02R(H02R), C02T(H02T), C02V(H02V), C02W(H02W), C02X(H02X), C02Z(H02Z),
 C032(H032), C033(H033), C035(H035), C036(H036), C038(H038), C039(H039),
 C03A(H03C), C03B(H03D), C03E(H03G), C03F(H03H), C03I(H03M), C03N(H03T),
 C03Q(H03Y), C03R(H03Z), C03U(H0AA), C03V(H1AA), C040(H040), C042(H042),
 C046(H046), C048(H048), C04B(H04E), C04E(H04Y), C04G(H04J), C04I(H04K),
 C04P(H5AA), C04U(H7AA), C04V(H04V), C04Y(H8AA), C052(H052), C12(H12)
6.d Idealised Me refined as rotating group:
 C04H(H04Z,HC,HD), C04K(H04,HE,HF), C04O(H4AA,HG,HH), C04S(H6AA,HI,HJ),
 C055(H05Q,H05R,H05S), C059(H05T,H05U,H05V), C05A(H05K,H05L,H05M), C05E(H05N,
 H05O,H05P), C05F(H05E,H05F,H05G), C05H(H05W,H05X,H05Y), C05I(H05H,H05I,H05J),
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              7114
_shelx_fab_checksum              89786
_platon_squeeze_void_probe_radius 1.20
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.830