Installation of Internal Electric Fields by Non-Redox Active Cations in Transition Metal Complexes
Kang, Kevin; Fuller, Jack; Reath, Alexander H.; Ziller, Joseph W.; Alexandrova, Anastassia; Yang, Jenny Y.; Chemical Science  (2019) –; doi:10.1039/C9SC02870F

data_1552308
_publ_section_title
;
 Installation of Internal Electric Fields by Non-Redox Active Cations in
 Transition Metal Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02870F
_journal_year                    2019
_chemical_formula_sum            'C50 H56 Ba2 F12 N4 Ni2 O26 S4'
_chemical_formula_weight         1877.32
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-11 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.3583(10)
_cell_angle_beta                 74.2611(11)
_cell_angle_gamma                79.4090(11)
_cell_formula_units_Z            1
_cell_length_a                   10.0313(10)
_cell_length_b                   12.0323(12)
_cell_length_c                   14.3201(14)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      2.28
_cell_volume                     1622.6(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART 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  0.0205
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.076
_diffrn_reflns_theta_min         1.735
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.016
_exptl_absorpt_correction_T_max  0.4318
_exptl_absorpt_correction_T_min  0.3734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.204
_refine_diff_density_max         0.676
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0259P)^2^+2.0921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7701
_reflns_number_total             7985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02870f2.cif
_cod_data_source_block           jyy150
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1552308
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.684
_exptl_absorpt_special_details
; 
Reflections not merged 
20048 Corrected reflections written to file jyy150s.hkl 
Estimated minimum and maximum transmission:  0.3734  0.4318 
The ratio (0.8648) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              29472