Characterization of Reactive Organometallic Species via MicroED.
Jones, Christopher G.; Asay, Matthew; Kim, Lee Joon; Kleinsasser, Jack F.; Saha, Ambarneil; Fulton, Tyler J.; Berkley, Kevin R.; Cascio, Duilio; Malyutin, Andrey G.; Conley, Matthew P.; Stoltz, Brian M.; Lavallo, Vincent; Rodríguez, José A; Nelson, Hosea M.; ACS central science 5 (2019) 1507–1513; doi:10.1021/acscentsci.9b00403

data_4514924
_publ_section_title
;
 Characterization of Reactive Organometallic Species via MicroED.
;
_journal_issue                   9
_journal_name_full               'ACS central science'
_journal_page_first              1507
_journal_page_last               1513
_journal_paper_doi               10.1021/acscentsci.9b00403
_journal_volume                  5
_journal_year                    2019
_chemical_formula_sum            'C38.51 H46.04 B18 Cl18 O2.49 P2 Pd2'
_chemical_formula_weight         1656.17
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   '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
_cell_angle_alpha                90
_cell_angle_beta                 91.4479(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4952(4)
_cell_length_b                   15.2588(4)
_cell_length_c                   27.3371(7)
_cell_measurement_reflns_used    9716
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.75
_cell_measurement_theta_min      2.37
_cell_volume                     6461.5(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL 2018/2 (XT)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            148833
_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         30.999
_diffrn_reflns_theta_min         1.873
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2012/1'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       blade
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         20596
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0243P)^2^+7.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16909
_reflns_number_total             20596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc9b00403_si_011.cif
_cod_data_source_block           vl334jk
_cod_database_code               4514924
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.645
_shelx_estimated_absorpt_t_max   0.794
_shelx_res_checksum              70156
_shelx_hkl_checksum              79627