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_7123881
_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         'C44 H46 Cr N2 P, C3 H7'
_chemical_formula_sum            'C47 H53 Cr N2 P'
_chemical_formula_weight         728.88
_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     dual
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-02 deposited with the CCDC.    2019-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.567(3)
_cell_angle_beta                 98.370(3)
_cell_angle_gamma                115.198(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3491(4)
_cell_length_b                   11.6086(4)
_cell_length_c                   17.2859(6)
_cell_measurement_reflns_used    16061
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.1260
_cell_measurement_theta_min      3.8520
_cell_volume                     1998.77(14)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     36.00  67.00   0.50    1.00    --   -9.50 -19.00-180.00   62
  2  \w    -53.00 -13.00   0.50    1.00    --   -9.50 -19.00-180.00   80
  3  \w    -33.00  29.00   0.50    1.00    --   -9.50 -82.00 150.00  124
  4  \w    -14.00  21.00   0.50    1.00    --   -9.50 -77.00 -60.00   70
  5  \w    -33.00  32.00   0.50    1.00    --   -9.50 -82.00  60.00  130
  6  \w    -58.00  16.00   0.50    1.00    --   -9.50 -57.00 -60.00  148
  7  \w    -28.00  97.00   0.50    1.00    --    9.50  38.00 -60.00  250
  8  \w    -72.00 -14.00   0.50    1.00    --    9.50 -57.00   0.00  116
  9  \w    -69.00  44.00   0.50    1.00    --    9.50 -38.00  60.00  226
;
_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      -0.0361346000
_diffrn_orient_matrix_UB_12      0.0054160000
_diffrn_orient_matrix_UB_13      -0.0353394000
_diffrn_orient_matrix_UB_21      -0.0604756000
_diffrn_orient_matrix_UB_22      -0.0330942000
_diffrn_orient_matrix_UB_23      0.0125095000
_diffrn_orient_matrix_UB_31      0.0064404000
_diffrn_orient_matrix_UB_32      0.0601613000
_diffrn_orient_matrix_UB_33      0.0196029000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.542
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83843
_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    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0556P)^2^+1.3772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6916
_reflns_number_total             7834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           5
_cod_original_cell_volume        1998.76(13)
_cod_database_code               7123881
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cr C H P N'
_chemical_oxdiff_usercomment     'XLH180517-7, Ybdma'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 99.45
_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), C43(H43a,H43b), C39(H39a,H39b), C37(H37a,H37b), C41(H41a,H41b),
 C47(H47a,H47b), C46(H46a,H46b)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C30(H30), C36(H36), C2(H2), C24(H24), C32(H32), C20(H20), C5(H5),
 C29(H29), C23(H23), C18(H18), C22(H22), C3(H3), C4(H4), C27(H27), C28(H28),
 C15(H15), C26(H26), C21(H21), C35(H35), C16(H16), C33(H33), C17(H17), C34(H34)
2.c Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C38(H38a,H38b,H38c), C40(H40a,H40b,H40c), C42(H42a,H42b,
 H42c), C45(H45a,H45b,H45c)
;
_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 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.759