Heterometallic Al6Zn12 nano-plate with π-conjugated ligand: synthesis and nonlinear absorption properties
Wang, San-Tai; Liu, Chen-Hui; Zheng, Chan; Li, De-Jing; Fang, Wei-Hui; Zhang, Jian; Chemical Communications  (2021) –; doi:10.1039/D1CC05919J

data_7129186
_publ_section_title
;
 Heterometallic Al6Zn12 nano-plate with \p-conjugated ligand: synthesis
 and nonlinear absorption properties
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05919J
_journal_year                    2021
_chemical_formula_moiety         '5(C156 H114 Al6 O66 Zn12), 12(C7 H8 O)'
_chemical_formula_sum            'C864 H666 Al30 O342 Zn60'
_chemical_formula_weight         21251.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.5215(5)
_cell_length_b                   60.4942(4)
_cell_length_c                   117.8414(10)
_cell_measurement_reflns_used    55396
_cell_measurement_temperature    100.0(7)
_cell_measurement_theta_max      48.7570
_cell_measurement_theta_min      2.2850
_cell_volume                     224708(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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      100.0(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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    -18.00  10.00   0.20    3.00    --  -51.40  19.00   0.00  140
  2  \w    -24.00  23.00   0.20    3.00    --  -51.40  19.00  60.00  235
  3  \w    -29.00  18.00   0.20    3.00    --  -51.40  62.00 165.00  235
  4  \w   -124.00 -33.00   0.20    3.00    --  -51.40 -77.00 -94.00  455
  5  \w   -124.00 -99.00   0.20    3.00    --  -51.40-125.00 -90.00  125
  6  \w   -118.00 -93.00   0.20    3.00    --  -51.40-125.00   0.00  125
  7  \w   -113.00 -82.00   0.20    3.00    --  -51.40-125.00-180.00  155
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0035526000
_diffrn_orient_matrix_UB_12      -0.0157957000
_diffrn_orient_matrix_UB_13      0.0079048000
_diffrn_orient_matrix_UB_21      0.0304179000
_diffrn_orient_matrix_UB_22      0.0097846000
_diffrn_orient_matrix_UB_23      0.0061365000
_diffrn_orient_matrix_UB_31      -0.0294524000
_diffrn_orient_matrix_UB_32      0.0120323000
_diffrn_orient_matrix_UB_33      0.0053828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       132
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            152318
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        48.899
_diffrn_reflns_theta_max         48.899
_diffrn_reflns_theta_min         2.132
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             86208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2893
_refine_ls_number_reflns         41166
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+839.7795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29277
_reflns_number_total             41166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05919j2.cif
_cod_data_source_block           AlOC-57
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7129186
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C O Al Zn'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.820
_diffrn_oxdiff_digest_frames
;
013ac1f3296043fb61bf2a9f5f8869b18a014709748
;
_diffrn_oxdiff_digest_hkl
;
0160f4ee228710adb929988fa76865d91d751a
;
_reflns_odcompleteness_completeness 72.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8, H33 of O33, H34 of O34, H18 of O18, H24 of O24,
  H3 of O3, H51 of O51, H53a of O53, H67 of O67, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H87 of O87, H76 of O76, H86a of O86
2. Uiso/Uaniso restraints and constraints
Uanis(C165) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C166) \\sim Ueq,
Uanis(C163) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O86) \\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C159) \\sim Ueq, Uanis(C204)
\\sim Ueq, Uanis(C213) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C212) \\sim Ueq,
Uanis(C211) \\sim Ueq, Uanis(C210) \\sim Ueq, Uanis(C209) \\sim Ueq,
Uanis(C207) \\sim Ueq, Uanis(C213) \\sim Ueq, Uanis(C162) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O3(H3), O8(H8), O18(H18), O24(H24), O33(H33), O34(H34), O51(H51), O53(H53a),
 O67(H67), C92(H92a,H92b,H92c), C103(H10a,H10b,H10c), C150(H15a,H15b,H15c),
 O86(H86a), C164(H164), C165(H165), C172(H17g,H17h,H17i), C177(H17d,H17e,H17f),
 C179(H17a,H17b,H17c), C183(H18g,H18h,H18i), C184(H18d,H18e,H18f), C185(H18a,
 H18b,H18c), C196(H19a,H19b,H19c), C197(H19d,H19e,H19f), C198(H19g,H19h,H19i),
 C200(H20a,H20b,H20c), C201(H20l,H20m), C204(H20d,H20e,H20f), C205(H20g,H20h,
 H20i), C207(H20j,H20k), O87(H87)
3.b Secondary CH2 refined with riding coordinates:
 C137(H13a,H13b)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C21(H21), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34a),
 C35(H35), C36(H36), C38(H38), C41(H41), C43(H43), C44(H44), C45(H45), C49(H49),
  C50(H50), C52(H52), C53(H53), C55(H55), C59(H59), C60(H60), C63(H63),
 C65(H65), C66(H66), C71(H71), C73(H73), C74(H74), C75(H75), C80(H80), C82(H82),
  C83(H83), C84(H84), C86(H86), C88(H88), C89(H89), C91(H91), C94(H94),
 C96(H96), C99(H99), C105(H105), C106(H106), C107(H107), C108(H108), C112(H112),
  C114(H114), C115(H115), C118(H118), C121(H121), C122(H122), C124(H124),
 C126(H126), C130(H130), C133(H133), C134(H134), C136(H136), C143(H143),
 C145(H145), C146(H146), C147(H147), C148(H148), C149(H149), C151(H151),
 C152(H152), C156(H156), C157(H157), C158(H158), C159(H159), C160(H160),
 C161(H161), C163(H163), C166(H166), C167(H167), C168(H168), C170(H170),
 C171(H171), C173(H173), C175(H175), C176(H176), C178(H178), C180(H180),
 C181(H181), C182(H182), C186(H186), C187(H187), C188(H188), C190(H190),
 C191(H191), C192(H192), C193(H193), C194(H194), C195(H195), C199(H199),
 C202(H202), C203(H203), C206(H206), C208(H208), C209(H209), C210(H210),
 C211(H211), C213(H213), C214(H214), C215(H215), C216(H216)
3.d Fitted hexagon refined as free rotating group:
 C162(C163,C164,C165,C166,C167), C208(C209,C210,C211,C212,C213)
3.e Idealised tetrahedral OH refined as rotating group:
 O76(H76)
;
_shelx_res_checksum              42053
_shelx_fab_checksum              35168
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.870