Expanding the Series of Alkali Metal Plumbolyl Complexes to Na and K
Diaz-Rodriguez, Roberto; Kitos, Alexandros; Murugesu, Muralee; Dalton Transactions  (2022) –; doi:10.1039/D2DT02615E

data_7711283
_publ_section_title
;
 Expanding the Series of Alkali Metal Plumbolyl Complexes to Na and K
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02615E
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H120 K4 O8 Pb2 Si4'
_chemical_formula_sum            'C72 H120 K4 O8 Pb2 Si4'
_chemical_formula_weight         1796.81
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-03
_audit_creation_method
;
FinalCif V105 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.382(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9985(5)
_cell_length_b                   14.6914(5)
_cell_length_c                   20.5549(7)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    150
_cell_measurement_theta_max      55.517
_cell_measurement_theta_min      3.288
_cell_volume                     4226.0(3)
_computing_cell_refinement
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65629
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.920
_diffrn_reflns_theta_min         2.617
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    6.914
_exptl_absorpt_correction_T_max  0.0927
_exptl_absorpt_correction_T_min  0.0207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1233 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.2233.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Alkanes/1,2-dimethoxyethane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.070(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         15909
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0265P)^2^+0.3102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.947
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                14130
_reflns_number_total             15909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02615e2.cif
_cod_data_source_block           muru412
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7711283
_shelx_shelxl_version_number     2019/1
_olex2_exptl_crystal_mounting_method 'mounted on  cryoloop'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.930(7)
 0.070(7)
2. 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
3. Uiso/Uaniso restraints and constraints
O1 \\sim C69A \\sim C69B \\sim C70A \\sim C70B \\sim O2: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C69A) = Uanis(C69B)
Uanis(C70A) = Uanis(C70B)
4. Others
 Sof(C69B)=Sof(H69C)=Sof(H69D)=Sof(C70B)=Sof(H70C)=Sof(H70D)=1-FVAR(1)
 Sof(C69A)=Sof(H69A)=Sof(H69B)=Sof(C70A)=Sof(H70A)=Sof(H70B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A,H34B), C65(H65A,
 H65B), C66(H66A,H66B), C69A(H69A,H69B), C70A(H70A,H70B), C69B(H69C,H69D),
 C70B(H70C,H70D)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_olex2_submission_original_sample_id RDA159
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.312
_shelx_estimated_absorpt_t_max   0.608
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_shelx_res_checksum              87945
_shelx_hkl_checksum              93430