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_4086305
_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         'C11 H19 Cl Cr N2'
_chemical_formula_sum            'C11 H19 Cl Cr N2'
_chemical_formula_weight         266.73
_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
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0142(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4820(2)
_cell_length_b                   15.2516(3)
_cell_length_c                   11.2717(2)
_cell_measurement_reflns_used    1567
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.948
_cell_measurement_theta_min      5.802
_cell_volume                     1281.32(5)
_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      173.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_unetI/netI     0.1895
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9384
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.258
_diffrn_reflns_theta_min         4.891
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.018
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0842 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.7294.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.783
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.783
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1111
_reflns_number_total             2323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00661_si_002.cif
_cod_data_source_block           rjs
_cod_database_code               4086305
_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:
 C10(H10), C7(H7), C11(H11), C4(H4), C1(H1), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              66526
_shelx_hkl_checksum              68752
_olex2_submission_special_instructions 'No special instructions were received'