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_7123882
_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         'C104 H160 K4 P4'
_chemical_formula_sum            'C104 H160 K4 P4'
_chemical_formula_weight         1690.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-08-03
_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                90
_cell_angle_beta                 91.440(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0786(4)
_cell_length_b                   24.3001(5)
_cell_length_c                   21.1776(4)
_cell_measurement_reflns_used    49839
_cell_measurement_temperature    179.98(11)
_cell_measurement_theta_max      29.9830
_cell_measurement_theta_min      3.6070
_cell_volume                     10844.0(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.949
_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      3.00  29.00   0.50   16.00    --   -5.70  57.00  90.00   52
  2  \w    -35.00  25.00   0.50   16.00    --   -5.70  38.00 150.00  120
  3  \w    -31.00  -5.00   0.50   16.00    --   -5.70 -19.00 -90.00   52
  4  \w    -95.00  39.00   0.50   16.00    --   -5.70 -19.00 150.00  268
  5  \w    -22.00  32.00   0.50   16.00    --   -5.70 -82.00-120.00  108
  6  \w    -20.00  57.00   0.50   16.00    --    6.00  57.00-180.00  154
  7  \w      8.00  34.00   0.50   16.00    --    6.00  38.00  90.00   52
  8  \w    -21.00  95.00   0.50   16.00    --    6.00  38.00  60.00  232
  9  \w    -12.00  42.00   0.50   16.00    --    6.00 -82.00-120.00  108
 10  \w    -19.00  13.00   0.50   16.00    --    6.00 -82.00  30.00   64
;
_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      -0.0012489000
_diffrn_orient_matrix_UB_12      -0.0288019000
_diffrn_orient_matrix_UB_13      0.0052349000
_diffrn_orient_matrix_UB_21      0.0253540000
_diffrn_orient_matrix_UB_22      0.0022095000
_diffrn_orient_matrix_UB_23      0.0224986000
_diffrn_orient_matrix_UB_31      -0.0220958000
_diffrn_orient_matrix_UB_32      0.0041685000
_diffrn_orient_matrix_UB_33      0.0242808000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            188963
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79709
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         20261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0941P)^2^+16.1789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17211
_reflns_number_total             20261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           exp_1602_sq
_cod_database_code               7123882
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H P K'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 99.73
_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:
 C22(H22), C25(H25), C48(H48), C51(H51), C74(H74), C77(H77), C100(H100),
 C103(H103)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C33(H33A,H33B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
  C59(H59A,H59B), C65(H65A,H65B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,
 H71B), C85(H85A,H85B), C91(H91A,H91B), C93(H93A,H93B), C95(H95A,H95B),
 C97(H97A,H97B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C28(H28), C29(H29), C30(H30), C31(H31),
 C54(H54), C55(H55), C56(H56), C57(H57), C80(H80), C81(H81), C82(H82), C83(H83)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C92(H92A,H92B,H92C), C94(H94A,H94B,
 H94C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I)
;
_shelx_res_checksum              93409
_shelx_fab_checksum              61091
_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 1.811
_oxdiff_exptl_absorpt_empirical_full_min 0.790