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_7123884
_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         'C96 H108 Cr3 N6 P3'
_chemical_formula_sum            'C96 H108 Cr3 N6 P3'
_chemical_formula_weight         1594.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-08-08 deposited with the CCDC.    2019-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.826(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.5505(5)
_cell_length_b                   17.7159(2)
_cell_length_c                   41.6344(5)
_cell_measurement_reflns_used    48555
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      28.5680
_cell_measurement_theta_min      3.6080
_cell_volume                     19559.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_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    -57.00 -10.64   0.38    3.50    --  -15.70  77.00  60.00  122
  2  \w    -21.00  23.08   0.38    3.50    --  -15.70 -82.00 -90.00  116
  3  \w    -42.00  66.30   0.38    3.50    --  -15.70  57.00 -90.00  285
  4  \w    -26.00  54.18   0.38    3.50    --   15.80 -82.00 150.00  211
  5  \w    -12.00 101.24   0.38    3.50    --   15.80  57.00  30.00  298
  6  \w    -33.24  61.00   0.38    3.50    --   15.80 -82.00-180.00  248
  7  \w    -74.00  19.86   0.38    3.50    --   15.80 -57.00  90.00  247
;
_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      -0.0000435000
_diffrn_orient_matrix_UB_12      -0.0017376000
_diffrn_orient_matrix_UB_13      0.0170118000
_diffrn_orient_matrix_UB_21      -0.0234390000
_diffrn_orient_matrix_UB_22      -0.0192883000
_diffrn_orient_matrix_UB_23      -0.0011204000
_diffrn_orient_matrix_UB_31      0.0129066000
_diffrn_orient_matrix_UB_32      -0.0350449000
_diffrn_orient_matrix_UB_33      -0.0002251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            117360
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         22324
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+36.8533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                16294
_reflns_number_total             22324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           exp_1393
_cod_database_code               7123884
_chemical_oxdiff_formula         'Cr Cl C H P N'
_reflns_odcompleteness_completeness 99.72
_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. Restrained distances
 C13-C14
 1.38 with sigma of 0.005
 C16-C17
 1.38 with sigma of 0.02
 C15-C14
 1.38 with sigma of 0.005
 C17-C15
 2.38 with sigma of 0.005
3. Rigid bond restraints
 C14, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C62) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B),
 C39(H39A,H39B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B),
  C71(H71A,H71B), C89(H89A,H89B), C91(H91A,H91B), C93(H93A,H93B), C95(H95A,H95B)
5.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), C34(H34), C35(H35),
  C36(H36), C37(H37), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C66(H66), C67(H67), C68(H68),
  C69(H69), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C),
 C96(H96A,H96B,H96C)
;
_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 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.519