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_7243396
_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 Mo O5, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C41 H72 K2 Mo N4 O17'
_chemical_formula_weight         1067.16
_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
_audit_creation_date             2021-02-02
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-02 deposited with the CCDC.	2021-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                64.679(2)
_cell_angle_beta                 68.734(2)
_cell_angle_gamma                88.596(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8840(3)
_cell_length_b                   11.6242(3)
_cell_length_c                   12.7269(3)
_cell_measurement_reflns_used    12037
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.0830
_cell_measurement_theta_min      4.1590
_cell_volume                     1339.97(7)
_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 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.994
_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     25.00  88.00   0.50    0.50    --   45.50 -57.00-120.00  126
  2  \w    -20.00   6.00   0.50    0.50    --   45.50 -57.00 120.00   52
  3  \w     31.00  57.00   0.50    0.50    --   45.50 -57.00 120.00   52
  4  \w    -32.00  -4.00   0.50    0.50    --   45.50 -57.00  30.00   56
  5  \w    -42.00  -3.00   0.50    0.50    --   45.50 -57.00-120.00   78
  6  \w      2.00 134.00   0.50    0.50    --   45.50  77.00-150.00  264
  7  \w      9.00  89.00   0.50    0.50    --   45.50 -57.00  30.00  160
  8  \w     44.00 133.00   0.50    0.50    --   45.50  57.00 -60.00  178
  9  \w     21.00  52.00   0.50    0.57    --  100.10  15.00  30.00   62
 10  \w     87.00 113.00   0.50    0.57    --  100.10 -82.00  60.00   52
 11  \w     12.00 105.00   0.50    0.57    --  100.10 -82.00 -60.00  186
 12  \w    111.00 143.00   0.50    0.57    --  100.10 -82.00 -60.00   64
 13  \w     20.00  94.00   0.50    0.57    --  100.10  30.00-180.00  148
 14  \w    102.00 148.00   0.50    0.57    --  100.10  30.00-180.00   92
 15  \w     18.00 140.00   0.50    0.57    --  100.10 -82.00-180.00  244
 16  \w     45.00  96.00   0.50    0.57    --  100.10 -82.00-120.00  102
 17  \w     19.00 147.00   0.50    0.57    --  100.10 -82.00  30.00  256
 18  \w     27.00  76.00   0.50    0.57    --  100.10 -61.00-180.00   98
 19  \w     93.00 131.00   0.50    0.57    --  100.10 -61.00-120.00   76
 20  \w     12.00  79.00   0.50    0.57    --  100.10 -61.00-120.00  134
 21  \w    112.00 184.00   0.50    0.57    --  100.10  15.00  30.00  144
 22  \w     15.00 121.00   0.50    0.57    --  100.10 -82.00   0.00  212
 23  \w     61.00  94.00   0.50    0.57    --  100.10  15.00  30.00   66
 24  \w     73.00 105.00   0.50    0.57    --  100.10 -82.00 150.00   64
 25  \w     17.00 189.00   0.50    0.57    --  100.10 -15.00 -30.00  344
;
_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      -0.0082502000
_diffrn_orient_matrix_UB_12      0.0844597000
_diffrn_orient_matrix_UB_13      -0.1284384000
_diffrn_orient_matrix_UB_21      0.1349463000
_diffrn_orient_matrix_UB_22      0.0809343000
_diffrn_orient_matrix_UB_23      -0.0443169000
_diffrn_orient_matrix_UB_31      0.0732086000
_diffrn_orient_matrix_UB_32      -0.0913371000
_diffrn_orient_matrix_UB_33      -0.0518176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13672
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         4.173
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85630
_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    1.322
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.285(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7011
_refine_ls_number_restraints     1707
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.0952P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6973
_reflns_number_total             7011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp01592c2.cif
_cod_data_source_block           Mo(CO)52-
_cod_database_code               7243396
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.715(10)
 0.285(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C34(H34A,H34B), C40(H40A,H40B), C22(H22A,
 H22B), C31(H31A,H31B), C32(H32A,H32B), C39(H39A,H39B), C11(H11A,H11B), C8(H8A,
 H8B), C12(H12A,H12B), C9(H9A,H9B), C16(H16A,H16B), C10(H10A,H10B), C18(H18A,
 H18B), C36(H36A,H36B), C24(H24A,H24B), C19(H19A,H19B), C21(H21A,H21B),
 C42(H42A,H42B), C20(H20A,H20B), C15(H15A,H15B), C37(H37A,H37B), C41(H41A,H41B),
  C17(H17A,H17B), C7(H7A,H7B), C30(H30A,H30B), C6(H6A,H6B), C38(H38A,H38B),
 C28(H28A,H28B), C23(H23A,H23B), C25(H25A,H25B), C14(H14A,H14B), C29(H29A,H29B),
  C13(H13A,H13B), C27(H27A,H27B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11076
_shelx_fab_checksum              97283
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.732