A dianionic C<sub>3</sub>-symmetric scorpionate: synthesis and coordination chemistry.
Tretiakov, Serhii; Damen, Johannes A. M.; Lutz, Martin; Moret, Marc-Etienne; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13549–13556; doi:10.1039/d0dt02601h

data_7705312
_publ_section_title
;
 A dianionic C<sub>3</sub>-symmetric scorpionate: synthesis and
 coordination chemistry.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13549
_journal_page_last               13556
_journal_paper_doi               10.1039/d0dt02601h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H48 K4 N6 P2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C57 H49.5 K4 N6.5 P2'
_chemical_formula_weight         1043.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-06-19 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.794(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0632(12)
_cell_length_b                   12.0672(10)
_cell_length_c                   42.305(4)
_cell_measurement_reflns_used    8927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      1.94
_cell_volume                     10190.0(14)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex3
_computing_data_reduction        'Eval15, TWINABS-2012/1'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            102232
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.686
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2012/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 9604 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.335(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         22187
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0498P)^2^+5.3544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.953
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                21465
_reflns_number_total             22187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02601h2.cif
_cod_data_source_block           l0897a
_cod_depositor_comments
'Adding full bibliography for 7705312--7705317.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C57 H49.50 K4 N6.50 P2'
_cod_database_code               7705312
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              43624