Electronic structures and properties of dianionic pentacarbonyls [TM(CO)5]2− (TM = Cr, Mo, W)
Pei, Gerui; Shu, Cong-Cong; Li, Mengyang; Sun, Zhong-Ming; Yang, Tao; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP01592C

data_7243395
_publ_section_title
;
 Electronic structures and properties of dianionic pentacarbonyls
 [TM(CO)5]2&#x2212; (TM = Cr, Mo, W)
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP01592C
_journal_year                    2021
_chemical_formula_moiety         'C5 Cr O5, 2(C18 H36 K N2 O6), C2 H8 N2'
_chemical_formula_sum            'C43 H80 Cr K2 N6 O17'
_chemical_formula_weight         1083.33
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                63.886(3)
_cell_angle_beta                 66.660(3)
_cell_angle_gamma                86.853(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9523(3)
_cell_length_b                   11.6300(4)
_cell_length_c                   12.6749(4)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.0880
_cell_measurement_theta_min      4.2670
_cell_volume                     1316.98(9)
_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      99.99(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     31.00  58.00   0.50    0.50    --    0.00  77.00  90.00   54
  2  \w     -8.00  35.00   0.50    0.50    --    0.00 -57.00  30.00   86
  3  \w     44.00  87.00   0.50    0.50    --    0.00  38.00  30.00   86
  4  \w    -40.00   9.00   0.50    0.50    --    0.00  77.00  90.00   98
  5  \w    -44.00   7.00   0.50    0.50    --    0.00  38.00  30.00  102
  6  \w    -86.00 -26.00   0.50    0.50    --    0.00 -57.00  30.00  120
  7  \w     79.00 105.00   0.50    0.64    --   98.20  45.00  90.00   52
  8  \w     92.00 139.00   0.50    0.64    --   98.20 -45.00  90.00   94
  9  \w     50.00  76.00   0.50    0.64    --   98.20 -82.00 -60.00   52
 10  \w     50.00 141.00   0.50    0.64    --   98.20 -82.00-180.00  182
 11  \w     97.00 124.00   0.50    0.64    --   98.20 -82.00-120.00   54
 12  \w    125.00 188.00   0.50    0.64    --   98.20  82.00 150.00  126
 13  \w    149.00 184.00   0.50    0.64    --   98.20  82.00  30.00   70
 14  \w      9.00 128.00   0.50    0.64    --   98.20 -61.00  90.00  238
 15  \w     37.00  82.00   0.50    0.64    --   98.20 -45.00  90.00   90
 16  \w     14.00  39.00   0.50    0.64    --   98.20  15.00 -30.00   50
 17  \w     83.00 143.00   0.50    0.64    --   98.20  82.00  30.00  120
 18  \w     22.00  48.00   0.50    0.64    --   98.20 -77.00-120.00   52
 19  \w     64.00 184.00   0.50    0.64    --   98.20  15.00 -30.00  240
 20  \w     35.00 108.00   0.50    0.64    --   98.20 -82.00   0.00  146
 21  \w    114.00 140.00   0.50    0.64    --   98.20 -82.00 -60.00   52
 22  \w     61.00  86.00   0.50    0.64    --   98.20 -82.00-120.00   50
 23  \w     10.00 127.00   0.50    0.64    --   98.20 -82.00  90.00  234
 24  \w     67.00 105.00   0.50    0.64    --   98.20 -82.00 -90.00   76
 25  \w     15.00 149.00   0.50    0.64    --   98.20 -30.00-150.00  268
;
_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      0.0660478000
_diffrn_orient_matrix_UB_12      0.1288314000
_diffrn_orient_matrix_UB_13      -0.0259326000
_diffrn_orient_matrix_UB_21      -0.1400117000
_diffrn_orient_matrix_UB_22      0.0381239000
_diffrn_orient_matrix_UB_23      0.0534075000
_diffrn_orient_matrix_UB_31      -0.0026932000
_diffrn_orient_matrix_UB_32      -0.0646441000
_diffrn_orient_matrix_UB_33      0.1364131000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.995
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11491
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.998
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         4.270
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41612
_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            brown
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.273(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6070
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+0.7919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5710
_reflns_number_total             6070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp01592c2.cif
_cod_data_source_block           scc
_cod_original_cell_volume        1316.98(8)
_cod_database_code               7243395
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.727(10)
 0.273(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C11(H11A,H11B), C41(H41A,H41B), C31(H31A,H31B), C35(H35A,
 H35B), C26(H26A,H26B), C32(H32A,H32B), C19(H19A,H19B), C21(H21A,H21B),
 C15(H15A,H15B), C7(H7A,H7B), C20(H20A,H20B), C33(H33A,H33B), C39(H39A,H39B),
 C27(H27A,H27B), C10(H10A,H10B), C29(H29A,H29B), C28(H28A,H28B), C37(H37A,H37B),
  C24(H24A,H24B), C25(H25A,H25B), C14(H14A,H14B), C9(H9A,H9B), C18(H18A,H18B),
 C23(H23A,H23B), C36(H36A,H36B), C17(H17A,H17B), C30(H30A,H30B), C40(H40A,H40B),
  C13(H13A,H13B), C8(H8A,H8B), C42(H42A,H42B), C6(H6A,H6B), C34(H34A,H34B),
 C22(H22A,H22B), C16(H16A,H16B), C12(H12A,H12B), C43(H43A,H43B)
3.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6C,H6D)
;
_shelx_res_checksum              82146
_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 2.962
_oxdiff_exptl_absorpt_empirical_full_min 0.421