Syntheses and solid-state structures of two cofacial (bis)dipyrrin dichromium complexes in different charge states
Carsch, Kurtis; Elder, Shelby E.; Dogutan, Dilek K.; Nocera, Daniel G.; Yang, Junyu; Zheng, Shao-Liang; Daniel, Timothy; Betley, Theodore A.; Acta Crystallographica Section C 77 (2021) 161–166; doi:10.1107/S2053229621001388

data_2022338
_publ_section_title
;
 Syntheses and solid-state structures of two cofacial (bis)dipyrrin
 dichromium complexes in different charge states
;
_journal_coeditor_code           YD3014
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              161
_journal_page_last               166
_journal_paper_doi               10.1107/S2053229621001388
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'K2 [Cr2 (C49 H56 N4 O1) Cl2 (C4 H8 O)3], 0.5C4 H10 O, 0.5C4 H8 O'
_chemical_formula_moiety
'2(K +), C49 H56 Cl2 Cr2 N4 O4 2-, 0.5(C4 H10 O), 0.5(C4 H8 O)'
_chemical_formula_sum            'C65 H89 Cl2 Cr2 K2 N4 O5'
_chemical_formula_weight         1259.50
_chemical_melting_point          ?
_chemical_name_common            K2tBudmxCr2Cl2
_chemical_name_systematic
;Dipotassium
di-\m-chlorido-{\m-2,2'-[(10,10-dimethyl-9<i>H</i>-xanthene-1,8-diyl)bis(5-<i>tert</i>-butyl-2<i>H</i>-pyrrol-2-ylidene)bis(methanylylidene)]bis(5-<i>tert</i>-butyl-1<i>H</i>-pyrrol-1-ide)-\k^4^<i>N</i>,<i>N</i>':<i>N</i>'',<i>N</i>'''}dichromium(I)--tetrahydrofuran--diethyl ether
(1/0/5/0.5)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.785(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.554(2)
_cell_length_b                   16.640(3)
_cell_length_c                   22.267(3)
_cell_measurement_reflns_used    9436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.95
_cell_volume                     6503.5(16)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
OLEX2 (Dolomanov <i>et al.</i>, 2009) and SHELXL2018 (Sheldrick,
2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            160364
_diffrn_reflns_theta_full        25.080
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         2.321
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.195
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.579
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         11484
_refine_ls_number_restraints     776
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+32.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                9406
_reflns_number_total             11484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3014sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        6503.3(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2022338
_shelx_hkl_checksum              54962
_shelx_res_checksum              76903
_cod_database_fobs_code 2022338