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_2022337
_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          '[Cr2 (C49 H56 N4 O1) Cl2], C4 H10 O1'
_chemical_formula_moiety         'C49 H56 Cl2 Cr2 N4 O1, C4 H10 O1'
_chemical_formula_sum            'C53 H66 Cl2 Cr2 N4 O2'
_chemical_formula_weight         965.99
_chemical_name_common            tBudmxCr2Cl2
_chemical_name_systematic
'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(II) diethyl ether monosolvate'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.074(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.917(3)
_cell_length_b                   13.299(2)
_cell_length_c                   27.554(4)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.33
_cell_volume                     5302.1(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76692
_diffrn_reflns_theta_full        25.041
_diffrn_reflns_theta_max         25.041
_diffrn_reflns_theta_min         1.428
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6930
_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    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.580
_refine_diff_density_min         -0.409
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         9361
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+9.8138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                7894
_reflns_number_total             9361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3014sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        5302.1(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2022337
_shelx_hkl_checksum              30051
_shelx_res_checksum              14179
_cod_database_fobs_code 2022337