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_4514925
_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_moiety         'C36 H40 B18 Cl18 O2 P2 Pd2, 2(C4 H8 O)'
_chemical_formula_sum            'C44 H56 B18 Cl18 O2 P2 Pd2'
_chemical_formula_weight         1612.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                107.57(3)
_cell_angle_beta                 91.15(3)
_cell_angle_gamma                123.19(3)
_cell_formula_units_Z            1
_cell_length_a                   13.050(3)
_cell_length_b                   12.040(2)
_cell_length_c                   13.060(3)
_cell_measurement_reflns_used    3713
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.627
_cell_measurement_theta_min      0.077
_cell_volume                     1592.4(10)
_computing_cell_refinement       'XSCALE XDS'
_computing_data_collection       TVIPS
_computing_data_reduction        XDSCONV
_computing_molecular_graphics    ShelxLe
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 32
_diffrn_measured_fraction_theta_full 0.809
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measurement_device_type  'Technai F-30'
_diffrn_measurement_method       'continuous rotation'
_diffrn_radiation_type           '300 KeV electrons'
_diffrn_radiation_wavelength     0.01969
_diffrn_reflns_av_R_equivalents  0.2173
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_Laue_measured_fraction_full 0.809
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23883
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        0.627
_diffrn_reflns_theta_max         0.627
_diffrn_reflns_theta_min         0.077
_diffrn_source                   'electron microscope FEG'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       'nano prism'
_exptl_crystal_F_000             279
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.0007
_exptl_crystal_size_min          0.0005
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       1362(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     557
_refine_ls_restrained_S_all      1.803
_refine_ls_R_factor_all          0.2155
_refine_ls_R_factor_gt           0.1822
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3798
_refine_ls_wR_factor_ref         0.4004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2839
_reflns_number_total             3713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc9b00403_si_004.cif
_cod_data_source_block           scaled_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_atom_sites_solution_secondary' value 'Difmap' changed to 'difmap'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1592.3(8)
_cod_database_code               4514925
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.0
_shelx_estimated_absorpt_t_max   0.0
_shelx_res_checksum              45468
_shelx_hkl_checksum              3381