Crystal structures of two novel iron isocyanides from the reaction of 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate({-}1)
Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S205698902101313X

data_2243953
_publ_section_title
;
 Crystal structures of two novel iron isocyanides from the reaction of
 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate({-}1)
;
_journal_coeditor_code           YZ2014
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205698902101313X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[K (C9 H8 N1) (C12 H24 O6)]'
_chemical_formula_moiety         'C21 H32 K N O6'
_chemical_formula_sum            'C21 H32 K N O6'
_chemical_formula_weight         433.57
_chemical_name_systematic
(7-Methylindolin-1-ido-\k<i>N</i>)(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^<i>O</i>)potassium
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.864(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.784(3)
_cell_length_b                   9.754(3)
_cell_length_c                   21.783(7)
_cell_measurement_reflns_used    937
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.80
_cell_volume                     2290.1(12)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al</i>., 1999)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21112
_diffrn_reflns_theta_full        25.076
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4071
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0838P)^2^+1.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1698
_reflns_number_gt                2902
_reflns_number_total             4071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2014sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243953
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              94741
_shelx_res_checksum              17682
_cod_database_fobs_code 2243953