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_7711284
_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_formula_moiety         'C44 H72 Na2 O4 Pb Si2'
_chemical_formula_sum            'C44 H72 Na2 O4 Pb Si2'
_chemical_formula_weight         974.36
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-14 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.770(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3878(17)
_cell_length_b                   10.5283(8)
_cell_length_c                   20.5795(16)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    203.15
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.31
_cell_volume                     4825.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      203.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            227692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.132
_diffrn_reflns_theta_min         1.829
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0781 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.7519.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_recrystallization_method
'Grown via slow diffusion of hexane layered on a solution of compound in toluene/THF mixture at -20 C'
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         13001
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+2.6507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10883
_reflns_number_total             13001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02615e2.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7711284
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.485
_shelx_estimated_absorpt_t_min   0.318
_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
2. Uiso/Uaniso restraints and constraints
O4 \\sim C44 \\sim C43 \\sim C42 \\sim C41: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O3 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O2 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O1 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C29(H29A,H29B), C38(H38A,H38B), C33(H33A,H33B), C41(H41A,
 H41B), C36(H36A,H36B), C30(H30A,H30B), C42(H42A,H42B), C34(H34A,H34B),
 C35(H35A,H35B), C32(H32A,H32B), C44(H44A,H44B), C39(H39A,H39B), C31(H31A,H31B),
  C40(H40A,H40B), C43(H43A,H43B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C16(H16), C10(H10), C13(H13), C15(H15), C14(H14), C7(H7),
 C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C18(H18A,H18B,
 H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C21(H21A,
 H21B,H21C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              70645
_shelx_hkl_checksum              56662
_olex2_date_sample_completion    2021-12-01
_olex2_date_sample_data_collection 2021-05-06
_olex2_date_sample_submission    2021-05-05
_olex2_exptl_crystal_mounting_method
'Crystal chosen cut from a larger cluster of interpenetrated crystals. Mounted on a 200 uM MicroLoop using Parabar 10312 oil'
_olex2_submission_original_sample_id RDA63-97_S0953
_olex2_submission_special_instructions 'No special instructions were received'