Contrasting the group 6 metal-metal bonding in sodium dichromate(ii) and sodium dimolybdate(ii) polymethyl complexes: synthetic, X-ray crystallographic and theoretical studies.
Campbell, Ross; Kennedy, Alan R.; McLellan, Ross; Robertson, Stuart D.; Sproules, Stephen; Mulvey, Robert E.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5650–5659; doi:10.1039/c6dt04644d

data_7041842
_publ_section_title
;
 Contrasting the group 6 metal-metal bonding in sodium dichromate(ii) and
 sodium dimolybdate(ii) polymethyl complexes: synthetic, X-ray
 crystallographic and theoretical studies.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5650
_journal_page_last               5659
_journal_paper_doi               10.1039/c6dt04644d
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C25 H69 Cr2 N6 Na3'
_chemical_formula_sum            'C25 H69 Cr2 N6 Na3'
_chemical_formula_weight         626.83
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-29 deposited with the CCDC.
2017-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5520(7)
_cell_length_b                   14.8524(6)
_cell_length_c                   18.5398(8)
_cell_measurement_reflns_used    5399
_cell_measurement_temperature    150.1
_cell_measurement_theta_max      30.0744
_cell_measurement_theta_min      2.9489
_cell_volume                     3731.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.1
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
  1 omega   64.00   89.00   1.0000   89.2200
omega____ theta____ kappa____ phi______ frames
    -       20.8078  179.0000   30.0000 25

  2 omega  -89.00   32.00   1.0000   89.2200
omega____ theta____ kappa____ phi______ frames
    -      -21.5890    0.0000   30.0000 121

  3 omega   -9.00   16.00   1.0000   89.2200
omega____ theta____ kappa____ phi______ frames
    -       20.8078   77.0000 -120.0000 25

  4 omega  -52.00   47.00   1.0000   89.2200
omega____ theta____ kappa____ phi______ frames
    -       20.8078  -37.0000  120.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0269727000
_diffrn_orient_matrix_UB_12      0.0308239000
_diffrn_orient_matrix_UB_13      -0.0216010000
_diffrn_orient_matrix_UB_21      0.0446323000
_diffrn_orient_matrix_UB_22      -0.0216428000
_diffrn_orient_matrix_UB_23      0.0098874000
_diffrn_orient_matrix_UB_31      -0.0046600000
_diffrn_orient_matrix_UB_32      -0.0293548000
_diffrn_orient_matrix_UB_33      -0.0299765000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22619
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.971
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2169 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.009(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9490
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0290P)^2^+0.2163P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                6618
_reflns_number_total             9490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04644d2.cif
_cod_data_source_block           rm08
_cod_depositor_comments
'Adding full bibliography for 7041842--7041844.cif.'
_cod_database_code               7041842
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 96.58
_reflns_odcompleteness_iscentric 0
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C20 = N5-C21 = N5-C22 = N6-C23 = N6-C24 = N6-C25
 1.48 with sigma of 0.01
 N5A-C20A = N5A-C21A = N5A-C22A = N6A-C24A = N6A-C25A = N6A-C23A
 1.48 with sigma of 0.01
 C22A-C23A = C22-C23 = C11-C10 = C10A-C11A
 1.53 with sigma of 0.01
 N1-C8 = N1-C9 = N1-C10 = N2-C11 = N2-C12 = N2-C13
 1.48 with sigma of 0.01
 N1-C8A = N1-C9A = N1-C10A = N2-C11A = N2-C12A = N2-C13A
 1.48 with sigma of 0.01
3. Rigid bond restraints
 N5, N6, C20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N2, C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
N1 \\sim N2 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(N5) = Uanis(N5A)
Uanis(N6) = Uanis(N6A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
5. Others
 Sof(C22A)=Sof(H26A)=Sof(H26B)=Sof(C23A)=Sof(H27A)=Sof(H27B)=Sof(N5A)=Sof(N6A)=
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C20A)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(N5)=Sof(N6)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 FVAR(1)
 Sof(C8A)=Sof(H8A1)=Sof(H8A2)=Sof(H8A3)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9A1)=Sof(H9A2)=Sof(H9A3)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(2)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C16(H16A,H16B), C17(H17A,H17B), C22(H22A,
 H22B), C23(H23A,H23B), C22A(H26A,H26B), C23A(H27A,H27B), C10A(H10C,H10D),
 C11A(H11C,H11D)
6.b Me refined with riding coordinates:
 C13A(H13D,H13E,H13F)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C21A(H21D,H21E,H21F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F),
 C20A(H20D,H20E,H20F), C8A(H8A1,H8A2,H8A3), C9A(H9A1,H9A2,H9A3), C12A(H12D,H12E,
 H12F)
;
_olex2_submission_original_sample_id RM08
_olex2_submission_special_instructions 'No special instructions were received'