A complex with nitrogen single, double, and triple bonds to the same chromium atom: synthesis, structure, and reactivity
Beaumier, Evan P.; Billow, Brennan S.; Singh, Amrendra K.; Biros, Shannon M.; Odom, Aaron L.; Chem. Sci. 7 (2016) 2532–; doi:10.1039/C5SC04608D

data_1542274
_publ_section_title
;
 A complex with nitrogen single, double, and triple bonds to the same
 chromium atom: synthesis, structure, and reactivity
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2532
_journal_paper_doi               10.1039/C5SC04608D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C23 H42 Cr N4 O'
_chemical_formula_sum            'C23 H42 Cr N4 O'
_chemical_formula_weight         442.60
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3071(9)
_cell_length_b                   27.649(2)
_cell_length_c                   18.4003(16)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.048
_cell_measurement_theta_min      2.365
_cell_volume                     5165.8(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45327
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         1.853
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.9219.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.311
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.058
_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     545
_refine_ls_number_reflns         10180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0652P)^2^+1.1701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7916
_reflns_number_total             10180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04608d2.cif
_cod_data_source_block           bisimide
_cod_depositor_comments
;
Adding full bibliography for 1542271--1542274.cif.

2019-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H84 Cr2 N8 O2'
_cod_original_formula_weight         885.21
_cod_original_formula_moiety         '2(C23 H42 Cr N4 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5165.7(8)
_cod_database_code               1542274
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14A(H14A), C11A(H11A), C5A(H5A), C8A(H8A), C16(H16), C13(H13), C10(H10),
 C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C2AA(H2AA), C0AA(H0AA), C6(H6), C5(H5), C4(H4),
 C3(H3), C2(H2)
2.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C12A(H12A,H12B,H12C), C13A(H13A,
 H13B,H13C), C20A(H20A,H20B,H20C), C19A(H19A,H19B,H19C), C21A(H21A,H21B,H21C),
 C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,
 H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C14(H14B,H14C,H14D), C15(H15D,
 H15E,H15F), C12(H12D,H12E,H12F), C11(H11B,H11C,H11D), C8(H8B,H8C,H8D), C9(H9A,
 H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C21(H21D,H21E,H21F)
;
_shelx_res_checksum              51825
_olex2_submission_special_instructions 'No special instructions were received'