Synthesis and reactivity of asymmetric Cr(I) dinitrogen complexes supported by cyclopentadienyl-phosphine ligands
Li, Jiapeng; Yin, Jianhao; Wang, Gao-Xiang; Yin, Zhu-Bao; Zhang, Wen-Xiong; Xi, Zhenfeng; Chemical Communications  (2019) –; doi:10.1039/C9CC02960E

data_7123875
_publ_section_title
;
 Synthesis and reactivity of asymmetric Cr(I) dinitrogen complexes
 supported by cyclopentadienyl-phosphine ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02960E
_journal_year                    2019
_chemical_formula_moiety         'C26 H40 Cl Cr P'
_chemical_formula_sum            'C26 H40 Cl Cr P'
_chemical_formula_weight         471.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-08 deposited with the CCDC.    2019-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                75.066(2)
_cell_angle_beta                 72.107(3)
_cell_angle_gamma                73.390(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0749(4)
_cell_length_b                   11.1730(3)
_cell_length_c                   11.5235(3)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    179.97(10)
_cell_measurement_theta_max      30.5520
_cell_measurement_theta_min      3.9500
_cell_volume                     1277.56(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9952
_diffrn_measured_fraction_theta_max 0.9952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  31.00   0.50    1.23    --   -1.60 -82.00   0.00  128
  2  \w      6.00  31.00   0.50    1.23    --   -1.60 -82.00  30.00   50
  3  \w    -33.00  30.00   0.50    1.23    --    1.90 -77.00 -90.00  126
  4  \w    -23.00  34.00   0.50    1.23    --    1.90 -82.00  60.00  114
  5  \w    -20.00  26.00   0.50    1.23    --    1.90 -19.00  90.00   92
  6  \w    -32.00  31.00   0.50    1.23    --    1.90 -82.00-150.00  126
  7  \w    -16.00  52.00   0.50    1.23    --    1.90  38.00  30.00  136
  8  \w     65.00  90.00   0.50    1.23    --    1.90  38.00  30.00   50
  9  \w    -81.00 -56.00   0.50    1.23    --    1.90 -19.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0079109000
_diffrn_orient_matrix_UB_12      -0.0640290000
_diffrn_orient_matrix_UB_13      -0.0045948000
_diffrn_orient_matrix_UB_21      0.0685776000
_diffrn_orient_matrix_UB_22      -0.0072314000
_diffrn_orient_matrix_UB_23      -0.0182516000
_diffrn_orient_matrix_UB_31      0.0022346000
_diffrn_orient_matrix_UB_32      -0.0198635000
_diffrn_orient_matrix_UB_33      0.0630853000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22696
_diffrn_reflns_theta_full        27.4806
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.2244
_exptl_crystal_description       block
_exptl_crystal_F_000             505.2842
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.6553
_refine_diff_density_min         -0.6080
_refine_diff_density_rms         0.0719
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             5.5413
_refine_ls_goodness_of_fit_ref   1.0321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0321
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.2827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5204
_reflns_number_total             5836
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           exp_1196
_cod_database_code               7123875
_chemical_oxdiff_formula         'Cr C H P N Cl'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C19(H19a,H19b), C21(H21a,H21b), C23(H23a,H23b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C26(H26a,
 H26b,H26c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.714