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_7123883
_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         'C128 H144 K4 P4'
_chemical_formula_sum            'C128 H144 K4 P4'
_chemical_formula_weight         1962.70
_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             2018-08-07
_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                113.944(4)
_cell_angle_beta                 100.357(3)
_cell_angle_gamma                108.053(3)
_cell_formula_units_Z            2
_cell_length_a                   17.9093(6)
_cell_length_b                   18.1403(8)
_cell_length_c                   20.5737(7)
_cell_measurement_reflns_used    15836
_cell_measurement_temperature    89.9(5)
_cell_measurement_theta_max      28.5170
_cell_measurement_theta_min      3.5830
_cell_volume                     5437.1(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      89.9(5)
_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    -96.00 -32.00   0.50    6.00    --  -15.70 -57.00-150.00  128
  2  \w    -15.00  14.00   0.50    6.00    --  -15.70 -82.00 -90.00   58
  3  \w    -44.00  68.00   0.50    6.00    --  -15.70  57.00 -60.00  224
  4  \w    -33.00  -3.00   0.50    6.00    --  -15.70 -82.00 120.00   60
  5  \w    -53.00 -12.00   0.50    6.00    --  -15.70  77.00  90.00   82
  6  \w    -10.00  40.00   0.50    6.00    --  -15.70  57.00   0.00  100
  7  \w    -74.00  36.00   0.50    6.00    --   15.80 -57.00 120.00  220
  8  \w    -34.00  61.00   0.50    6.00    --   15.80 -82.00-150.00  190
  9  \w    -11.00  85.00   0.50    6.00    --   15.80  57.00  60.00  192
;
_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      0.0221730000
_diffrn_orient_matrix_UB_12      0.0243694000
_diffrn_orient_matrix_UB_13      0.0397588000
_diffrn_orient_matrix_UB_21      0.0075295000
_diffrn_orient_matrix_UB_22      -0.0369001000
_diffrn_orient_matrix_UB_23      -0.0020502000
_diffrn_orient_matrix_UB_31      0.0378379000
_diffrn_orient_matrix_UB_32      0.0167428000
_diffrn_orient_matrix_UB_33      -0.0062273000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72066
_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         27.484
_diffrn_reflns_theta_min         3.438
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70510
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         24866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0750P)^2^+9.5294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16793
_reflns_number_total             24866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02960e2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        5437.1(4)
_cod_database_code               7123883
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cr1 Cl1 C1 P1 N1'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.65
_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:
 C00Q(H00A,H00B), C00S(H00C,H00D), C00Z(H00E,H00F), C01F(H01D,H01E), C01Q(H01F,
 H01G), C01X(H01H,H01I), C01Z(H01J,H01K), C02F(H02G,H02H), C02U(H02V,H02W),
 C02W(H02Y,H), C03H(H03J,H03K), C7(H7A,H7B), C020(H0AA,HB), C021(H1AA,HC),
 C022(H2AA,HD), C025(H3AA,HE), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B),
 C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00P(H00P), C00V(H00V), C01A(H01A), C01B(H01B), C01C(H01C),
 C01L(H01L), C01M(H01M), C01N(H01N), C01P(H01P), C01R(H01R), C01S(H01S),
 C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01Y(H01Y), C2(H2), C02B(H02D),
  C02D(H02E), C02E(H02F), C02I(H02L), C02K(H02M), C02L(H02N), C02P(H02U),
 C02V(H02X), C02Y(H02Z), C02Z(H02), C3(H3), C03E(H03G), C03F(H03H), C03G(H03I),
 C03I(H03L), C03L(H03P), C03M(H03Q), C4(H4), C5(H5), C010(H010), C14(H14),
 C15(H15), C016(H016), C16(H16), C17(H17), C18(H18), C019(H019), C20(H20),
 C21(H21), C22(H22), C23(H23), C023(H023), C24(H24), C028(H028), C029(H029),
 C030(H030), C033(H033), C037(H037)
2.c Idealised Me refined as rotating group:
 C02A(H02A,H02B,H02C), C02G(H02I,H02J,H02K), C02M(H02O,H02P,H02Q), C02O(H02R,
 H02S,H02T), C03C(H03A,H03B,H03C), C03D(H03D,H03E,H03F), C03K(H03M,H03N,H03O),
 C03O(H03R,H03S,H03T), C03Q(H03U,H03V,H03W), C03R(H03X,H03Y,HA), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C036(H03Z,HF,HG), C038(H03,HH,HI)
;
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.783