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_7241208
_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_formula_sum            'C176 H112 O41.42 Pb16'
_chemical_formula_weight         6204.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.8392(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.3686(18)
_cell_length_b                   10.8690(5)
_cell_length_c                   27.3181(13)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      42.8911
_cell_measurement_theta_min      2.9178
_cell_volume                     8293.5(7)
_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-2016/6 (Sheldrick, 2015, 2016), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            60989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    16.250
_exptl_absorpt_correction_T_max  0.1081
_exptl_absorpt_correction_T_min  0.0365
_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    2.485
_exptl_crystal_description       block
_exptl_crystal_F_000             5623
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.163
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         12660
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0134P)^2^+64.6381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11570
_reflns_number_total             12660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01150a2.cif
_cod_data_source_block           lead_oxide_2-naphthoate_hydrate(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7241208
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.101
_shelx_estimated_absorpt_t_max   0.246
_shelx_res_checksum              98821