A five-stranded heterometallic helicate.
Sudan, Sylvain; Fadaei-Tirani, Farzaneh; Severin, Kay; Chemical communications (Cambridge, England) 59 (2023) 8258–8261; doi:10.1039/d3cc02045b

data_7131797
_publ_section_title
;
 A five-stranded heterometallic helicate.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8258
_journal_page_last               8261
_journal_paper_doi               10.1039/d3cc02045b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C210 H155 La N12 O11 Pd2, 5[BF4]'
_chemical_formula_sum            'C210 H155 La N12 O11 Pd2'
_chemical_formula_weight         3374.16
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   30.9679(6)
_cell_length_b                   30.9679(6)
_cell_length_c                   34.1539(5)
_cell_measurement_reflns_used    19036
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      53.1760
_cell_measurement_theta_min      2.5590
_cell_volume                     28365.8(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (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  'ShelXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -74.00 -35.00   0.50   12.00    --  -67.15 100.00  -1.00   78
  2  \w    -55.00 -29.00   0.50   12.00    --  -69.26 128.00-161.00   52
  3  \w     57.00  96.00   0.50   12.00    --   69.47 158.00 162.00   78
  4  \w     35.00 103.00   0.50   12.00    --   78.01-128.00 124.00  136
  5  \w    -63.00 -37.00   0.50   12.00    --  -67.15 125.00-120.00   52
  6  \w   -106.00 -72.00   0.50   12.00    --  -69.26   0.00 -90.00   68
  7  \w     40.00  77.00   0.50   12.00    --   69.47 -95.00 -90.00   74
  8  \w     49.00  75.00   0.50   12.00    --   69.47 -95.00  60.00   52
  9  \w     33.00  76.00   0.50   12.00    --   69.47 -95.00 -60.00   86
 10  \w     29.00  95.00   0.50   12.00    --   69.47-125.00  90.00  132
 11  \w     42.00  78.00   0.50   12.00    --   78.01 -95.00-150.00   72
 12  \w     54.00 123.00   0.50   12.00    --   78.01  15.00 -60.00  138
 13  \w     75.00 115.00   0.50   12.00    --   78.01  15.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0543245000
_diffrn_orient_matrix_UB_12      -0.0149452000
_diffrn_orient_matrix_UB_13      0.0096075000
_diffrn_orient_matrix_UB_21      0.0184378000
_diffrn_orient_matrix_UB_22      0.0491332000
_diffrn_orient_matrix_UB_23      0.0227134000
_diffrn_orient_matrix_UB_31      -0.0026911000
_diffrn_orient_matrix_UB_32      0.0257006000
_diffrn_orient_matrix_UB_33      -0.0377872000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.1118
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            133335
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.591
_diffrn_reflns_theta_max         66.591
_diffrn_reflns_theta_min         2.587
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.704
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             10416
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2224
_refine_ls_number_reflns         33383
_refine_ls_number_restraints     4049
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1872
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1791P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2537
_refine_ls_wR_factor_ref         0.3158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14532
_reflns_number_total             33383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02045b2.cif
_cod_data_source_block           sy242
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        28365.8(12)
_cod_database_code               7131797
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         C210H155B5F20LaN12O11Pd2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C121-C120 = C122-C121 = C123-C122 = C224-C123 = C225-C224 = C225-C224 = C123-
 C122
 1.54 with sigma of 0.02
 C263-C162 = C264-C263 = C265-C264 = C265-C266 = C267-C266
 1.54 with sigma of 0.02
 C83-C82 = C82-C81 = C81-C80 = C80-C79 = C78-C79 = C37-C36 = C38-C37 = C39-C38
 = C40-C41 = C40-C39 = C205-C204 = C206-C205 = C207-C206 = C207-C208 = C209-
 C208 = C167-C166 = C165-C166 = C165-C164 = C164-C163 = C163-C162
 1.54 with sigma of 0.02
 C37-C36 = C38-C37 = C39-C38 = C40-C39 = C41-C40
 1.54 with sigma of 0.01
 C309-C308 = C308-C307 = C307-C306 = C306-C305 = C305-C304
 1.54 with sigma of 0.01
 C123-C224
 1.54 with sigma of 0.02
 C304-C175
 1.5 with sigma of 0.02
 C123-C122 = C223-C122 = C124-C123 = C125-C124 = C224-C223 = C225-C224
 1.54 with sigma of 0.01
 C264-C266 = C265-C267
 2.54 with sigma of 0.04
 C38-C40 = C39-C41 = C83-C81 = C82-C80
 2.54 with sigma of 0.04
 C162-C264 = C263-C265
 2.54 with sigma of 0.01
 C307-C309 = C308-C306
 2.54 with sigma of 0.04
 C225-C123 = C122-C224
 2.54 with sigma of 0.04
 C120-C122 = C121-C123 = C225-C123
 2.54 with sigma of 0.04
 C206-C208 = C207-C209
 2.54 with sigma of 0.04
 C37-C8 = C49-C79 = C80-C78 = C36-C38
 2.54 with sigma of 0.04
 C175-C205 = C204-C206
 2.54 with sigma of 0.04
 C133-C163 = C162-C164
 2.54 with sigma of 0.04
 C304-C306 = C307-C305
 2.54 with sigma of 0.04
 C265-C267
 2.54 with sigma of 0.01
 C266-C264
 2.54 with sigma of 0.01
 C264-C162
 2.54 with sigma of 0.01
 C162-C164
 2.54 with sigma of 0.01
 C164-C166 = C165-C167
 2.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
Uanis(C266) = Uanis(C267)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H12G)=Sof(H12H)=Sof(C223)=Sof(H22A)=Sof(H22B)=Sof(C224)=Sof(H22C)=
 Sof(H22D)=Sof(C225)=Sof(H22E)=Sof(H22F)=Sof(H22G)=1-FVAR(1)
 Sof(H12E)=Sof(H12F)=Sof(C123)=Sof(H12I)=Sof(H12J)=Sof(C124)=Sof(H12K)=
 Sof(H12L)=Sof(C125)=Sof(H12M)=Sof(H12N)=Sof(H12O)=FVAR(1)
 Sof(H16C)=Sof(H16D)=Sof(C263)=Sof(H26F)=Sof(H26G)=Sof(C264)=Sof(H26H)=
 Sof(H26I)=Sof(C265)=Sof(H26J)=Sof(H26K)=Sof(C266)=Sof(H26A)=Sof(H26B)=
 Sof(C267)=Sof(H26C)=Sof(H26D)=Sof(H26E)=1-FVAR(2)
 Sof(H16A)=Sof(H16B)=Sof(C163)=Sof(H16E)=Sof(H16F)=Sof(C164)=Sof(H16G)=
 Sof(H16H)=Sof(C165)=Sof(H16I)=Sof(H16J)=Sof(C166)=Sof(H16K)=Sof(H16L)=
 Sof(C167)=Sof(H16M)=Sof(H16N)=Sof(H16O)=FVAR(2)
 Sof(C304)=Sof(H30A)=Sof(H30B)=Sof(C305)=Sof(H30C)=Sof(H30D)=Sof(C306)=
 Sof(H30E)=Sof(H30F)=Sof(C307)=Sof(H30G)=Sof(H30H)=Sof(C308)=Sof(H30I)=
 Sof(H30J)=Sof(C309)=Sof(H30K)=Sof(H30L)=Sof(H30M)=1-FVAR(3)
 Sof(C204)=Sof(H20A)=Sof(H20B)=Sof(C205)=Sof(H20C)=Sof(H20D)=Sof(C206)=
 Sof(H20E)=Sof(H20F)=Sof(C207)=Sof(H20G)=Sof(H20H)=Sof(C208)=Sof(H20I)=
 Sof(H20J)=Sof(C209)=Sof(H20K)=Sof(H20L)=Sof(H20M)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C122(H12G,
 H12H), C123(H12I,H12J), C124(H12K,H12L), C162(H16A,H16B), C162(H16C,H16D),
 C163(H16E,H16F), C164(H16G,H16H), C165(H16I,H16J), C166(H16K,H16L), C204(H20A,
 H20B), C205(H20C,H20D), C206(H20E,H20F), C207(H20G,H20H), C208(H20I,H20J),
 C223(H22A,H22B), C224(H22C,H22D), C263(H26F,H26G), C264(H26H,H26I), C265(H26J,
 H26K), C266(H26A,H26B), C304(H30A,H30B), C305(H30C,H30D), C306(H30E,H30F),
 C307(H30G,H30H), C308(H30I,H30J)
6.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C83(H83A,H83B,H83C), C125(H12M,H12N,H12O), C167(H16M,
 H16N,H16O), C209(H20K,H20L,H20M), C225(H22E,H22F,H22G), C267(H26C,H26D,H26E),
 C309(H30K,H30L,H30M)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C18(H18), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C32(H32), C33(H33),
  C34(H34), C44(H44), C46(H46), C47(H47), C51(H51), C52(H52), C54(H54),
 C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C70(H70), C71(H71),
  C72(H72), C76(H76), C75(H75), C74(H74), C86(H86), C88(H88), C89(H89),
 C93(H93), C94(H94), C96(H96), C101(H101), C102(H102), C103(H103), C105(H105),
 C106(H106), C107(H107), C112(H112), C113(H113), C114(H114), C116(H116),
 C117(H117), C118(H118), C128(H128), C130(H130), C131(H131), C135(H135),
 C136(H136), C138(H138), C143(H143), C144(H144), C145(H145), C147(H147),
 C148(H148), C149(H149), C154(H154), C155(H155), C156(H156), C158(H158),
 C159(H159), C160(H160), C170(H170), C172(H172), C173(H173), C177(H177),
 C178(H178), C180(H180), C185(H185), C186(H186), C187(H187), C189(H189),
 C190(H190), C191(H191), C196(H196), C197(H197), C198(H198), C200(H200),
 C201(H201), C202(H202), C210(H210)
6.d Naphthalene refined as free rotating group:
 C69(C70,C71,C72,C73,C77,C76,N4,C75,C74)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33612
_shelx_hkl_checksum              89052
_shelx_fab_checksum              60852
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.901
_oxdiff_exptl_absorpt_empirical_full_min 0.668