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_7123880
_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         'C32 H36 Cl Cr P'
_chemical_formula_sum            'C32 H36 Cl Cr P'
_chemical_formula_weight         539.03
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                65.497(3)
_cell_angle_beta                 71.852(3)
_cell_angle_gamma                73.717(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4291(3)
_cell_length_b                   12.2337(3)
_cell_length_c                   13.0486(5)
_cell_measurement_reflns_used    11034
_cell_measurement_temperature    179.98(10)
_cell_measurement_theta_max      30.6310
_cell_measurement_theta_min      3.7360
_cell_volume                     1417.35(9)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  30.00   0.50    0.97    --   -1.60 -82.00   0.00  126
  2  \w    -33.00  25.00   0.50    0.97    --   -1.60 -82.00  60.00  116
  3  \w    -20.00   6.00   0.50    0.97    --   -1.60 -82.00  30.00   52
  4  \w     59.00  85.00   0.50    0.97    --    1.90  38.00   0.00   52
  5  \w    -13.00  50.00   0.50    0.97    --    1.90  38.00   0.00  126
  6  \w    -43.00 -14.00   0.50    0.97    --    1.90 -77.00 150.00   58
  7  \w     -5.00  31.00   0.50    0.97    --    1.90 -77.00 150.00   72
  8  \w    -26.00  33.00   0.50    0.97    --    1.90 -82.00 -90.00  118
  9  \w     23.00  49.00   0.50    0.97    --    1.90  57.00-150.00   52
 10  \w    -29.00  25.00   0.50    0.97    --    1.90 -82.00-150.00  108
;
_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      -0.0695833000
_diffrn_orient_matrix_UB_12      0.0042778000
_diffrn_orient_matrix_UB_13      0.0009602000
_diffrn_orient_matrix_UB_21      0.0204236000
_diffrn_orient_matrix_UB_22      -0.0100325000
_diffrn_orient_matrix_UB_23      -0.0530234000
_diffrn_orient_matrix_UB_31      0.0050171000
_diffrn_orient_matrix_UB_32      -0.0637889000
_diffrn_orient_matrix_UB_33      0.0307224000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24131
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.496
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88733
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0407P)^2^+0.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5708
_reflns_number_total             6463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           exp_1178
_cod_database_code               7123880
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cr1 C1 H1 P1 Cl1 N1'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 99.58
_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 Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C25(H25a,H25b), C27(H27a,H27b), C29(H29a,H29b), C31(H31a,H31b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C32(H32a,H32b,
 H32c)
;
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.735