Synthesis and Structure of Chromium(VI) Nitrido Cyclopentadienyl Complexes
Billow, Brennan S.; Bemowski, Ross D.; DiFranco, Stephen A.; Staples, Richard J.; Odom, Aaron L.; Organometallics 34 (2015) 4567–; doi:10.1021/acs.organomet.5b00661

data_4086303
_publ_section_title
;
 Synthesis and Structure of Chromium(VI) Nitrido Cyclopentadienyl
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4567
_journal_paper_doi               10.1021/acs.organomet.5b00661
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C17 H33 Cr N3'
_chemical_formula_sum            'C17 H33 Cr N3'
_chemical_formula_weight         331.46
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4468(3)
_cell_length_b                   18.9011(8)
_cell_length_c                   13.5482(6)
_cell_measurement_reflns_used    8838
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.291
_cell_measurement_theta_min      2.155
_cell_volume                     1901.14(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_laue_measured_fraction_full 0.976
_diffrn_reflns_laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11529
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.315
_diffrn_reflns_theta_min         1.853
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0944 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.5470.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            dark
_exptl_crystal_colour_modifier   dark
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       irregular
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.805
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0626P)^2^+0.6867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3136
_reflns_number_total             3374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00661_si_002.cif
_cod_data_source_block           sd09feb2010_0m
_cod_database_code               4086303
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.643
_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:
 C22(H22), C31(H31), C32(H32), C21(H21), C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C211(H21A,H21B,H21C), C311(H31A,H31B,H31C), C222(H22A,H22B,H22C), C321(H32A,
 H32B,H32C), C312(H31D,H31E,H31F), C322(H32D,H32E,H32F), C221(H22D,H22E,H22F),
 C212(H21D,H21E,H21F)
;
_shelx_res_checksum              49817
_shelx_hkl_checksum              83550
_olex2_submission_special_instructions 'No special instructions were received'