Ligand Geometry Directs the Packing and Symmetry of One-Dimensional Helical Motifs in Lead Oxide Naphthoates and Biphenylcarboxylates
Hammer, Arden C.; Jia, Xiwen; Zeller, Matthias; Coughlin, Ezra John; Zhang, Weiguo; Oertel, Catherine M.; CrystEngComm  (2020) –; doi:10.1039/D0CE01150A

data_7241209
_publ_section_title
;
 Ligand Geometry Directs the Packing and Symmetry of One-Dimensional
 Helical Motifs in Lead Oxide Naphthoates and Biphenylcarboxylates
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01150A
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26 H18 O5 Pb2'
_chemical_formula_weight         824.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.255(3)
_cell_length_b                   21.255(3)
_cell_length_c                   10.8720(8)
_cell_measurement_reflns_used    9139
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.8195
_cell_measurement_theta_min      2.8444
_cell_volume                     4911.7(10)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2018/1 (Sheldrick, 2015, 2017), 
SHELXLE Rev882 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41140
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.642
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.669
_diffrn_reflns_theta_min         2.846
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    13.726
_exptl_absorpt_correction_T_max  0.4958
_exptl_absorpt_correction_T_min  0.2489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_description       needle
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Flack x determined using 2824 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         12530
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.389
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.376
_reflns_number_gt                8699
_reflns_number_total             12530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01150a2.cif
_cod_data_source_block           lead_oxide_biphenyl-3-carboxylate(5)
_cod_original_cell_volume        4911.9(12)
_cod_database_code               7241209
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.055
_shelx_estimated_absorpt_t_max   0.771
_shelx_res_checksum              72784