Pushing the Limits of Delta Bonding in Metal-Chromium Complexes with Redox Changes and Metal Swapping.
Eisenhart, Reed J.; Rudd, P. Alex; Planas, Nora; Boyce, David W.; Carlson, Rebecca K.; Tolman, William B.; Bill, Eckhard; Gagliardi, Laura; Lu, Connie C.; Inorganic chemistry 54 (2015) 7579–7592; doi:10.1021/acs.inorgchem.5b01163

data_4343898
_publ_section_title
;
 Pushing the Limits of Delta Bonding in Metal-Chromium Complexes with
 Redox Changes and Metal Swapping.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7579
_journal_page_last               7592
_journal_paper_doi               10.1021/acs.inorgchem.5b01163
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C39 H60 Cr Mn N4 P3, C18 H36 K N2 O6'
_chemical_formula_sum            'C57 H96 Cr K Mn N6 O6 P3'
_chemical_formula_weight         1200.35
_chemical_name_common            'LCrMn2.2.2 CryptK'
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   11.3119(7)
_cell_length_b                   11.3119(7)
_cell_length_c                   28.5164(18)
_cell_measurement_reflns_used    16242
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.184
_cell_volume                     3160.1(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.079
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0365P)^2^+0.7111P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4397
_reflns_number_total             4850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01163_si_002.cif
_cod_data_source_block           12219rje_ComplexK222[3red]
_cod_depositor_comments
;Adding full bibliography for 4343895--4343899.cif.

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3160.1(4)
_cod_database_code               4343898
_shelxl_version_number           2013-2
_shelx_res_checksum              33916
_shelx_hkl_checksum              33151