The structure of a pentachromium(II) extended metal atom chain at 3 K: Cotton’s conjecture proven
Cornia, Andrea; Nicolini, Alessio; McMonagle, Charles J.; Probert, Michael; Dalton Transactions  (2022) –; doi:10.1039/D2DT03103E

data_7711666
_publ_section_title
;
 The structure of a pentachromium(II) extended metal atom chain at 3 K:
 Cotton&#x2019;s conjecture proven
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03103E
_journal_year                    2022
_chemical_compound_source        synthesis
_chemical_formula_iupac          '[Cr5(C15H11N5)4(NCS)2]'
_chemical_formula_moiety         'C62 H44 Cr5 N22 S2'
_chemical_formula_sum            'C62 H44 Cr5 N22 S2'
_chemical_formula_weight         1421.31
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-17
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-21 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2426(3)
_cell_length_b                   26.2039(7)
_cell_length_c                   15.2056(3)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    291.8
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.67
_cell_volume                     6073.4(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_publication_material
'WINGX publication routines v2020.2 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      291.8
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device       'four-circle Huber diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5213
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.546
_diffrn_source                   'rotating anode'
_diffrn_source_current           108.0
_diffrn_source_power             5.4
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.639976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
Final HKLF 4 output contains 28556 reflections, Rint = 0.0347
(12553 with I > 3sig(I), Rint = 0.0303)
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             2888
_exptl_crystal_preparation
'Et2O vapour diffusion into a CH2Cl2 solution,Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/CH2Cl2'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0570P)^2^+6.2666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3680
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03103e2.cif
_cod_data_source_block           ambient_after
_cod_database_code               7711666
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.789
_shelx_res_checksum              58884
_shelx_hkl_checksum              53173