Electronic Coupling between Two Covalently Bonded Dimolybdenum Units Bridged by a Naphthalene Group.
Zhu, Guang Yuan; Meng, Miao; Tan, Ying Ning; Xiao, Xuan; Liu, Chun Y.; Inorganic chemistry 55 (2016) 6315–6322; doi:10.1021/acs.inorgchem.6b01021

data_4348153
_publ_section_title
;
 Electronic Coupling between Two Covalently Bonded Dimolybdenum Units
 Bridged by a Naphthalene Group.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6315
_journal_page_last               6322
_journal_paper_doi               10.1021/acs.inorgchem.6b01021
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C102 H96 Mo4 N12 O12 S4, C4 O2'
_chemical_formula_sum            'C102 H96 Mo4 N12 O12 S4'
_chemical_formula_weight         2193.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                92.208(3)
_cell_angle_beta                 99.738(3)
_cell_angle_gamma                100.073(4)
_cell_formula_units_Z            1
_cell_length_a                   9.6079(4)
_cell_length_b                   12.7804(6)
_cell_length_c                   20.3393(8)
_cell_measurement_reflns_used    5971
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      62.8920
_cell_measurement_theta_min      4.0260
_cell_volume                     2417.61(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -36.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184  -57.0000   90.0000 89

  2 omega   71.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -91.0000   46.5460 27

  3 omega   72.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -12.7996 28

  4 omega   76.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000 -100.8891 27

  5 omega   68.00  163.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000    0.0000 95

  6 omega  109.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000   30.0000 35

  7 omega  128.00  155.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000 -120.0000 27

  8 omega   69.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000 -120.0000 31

  9 omega   62.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   57.0000 -120.0000 40

 10 omega   39.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -120.0000 29

 11 omega   22.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -60.0000 52

 12 omega   40.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -48.3362 74

 13 omega   40.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -91.0000   46.5460 26

 14 omega   23.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000  -30.0000 46

 15 omega   24.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000   60.0000 52

 16 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000   90.0000 34

 17 omega   29.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000  150.0000 32

 18 omega   46.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -89.0000  144.5747 59

 19 omega   23.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000   77.2331 93

 20 omega   40.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000 -100.8891 32

 21 omega   24.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -150.0000 44

 22 omega   19.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000 -160.1966 91

 23 omega   18.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000    0.0000 37

 24 omega  -21.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184  -99.0000 -150.0000 96

 25 omega  -27.00   57.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184  -96.0000  -13.0000 84

 26 omega  -89.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184  -57.0000    0.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0473913000
_diffrn_orient_matrix_UB_12      0.0657052000
_diffrn_orient_matrix_UB_13      0.0544856000
_diffrn_orient_matrix_UB_21      0.1430493000
_diffrn_orient_matrix_UB_22      -0.0016795000
_diffrn_orient_matrix_UB_23      0.0470875000
_diffrn_orient_matrix_UB_31      0.0684655000
_diffrn_orient_matrix_UB_32      0.1036475000
_diffrn_orient_matrix_UB_33      -0.0273737000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15125
_diffrn_reflns_theta_full        62.77
_diffrn_reflns_theta_max         62.77
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         7623
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.4072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                6152
_reflns_number_total             7623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01021_si_002.cif
_cod_data_source_block           S2-naph-S2
_cod_original_cell_volume        2417.63(18)
_cod_database_code               4348153
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1S-C2S = C3S-C4S
 1.53 with sigma of 0.02
 C2S-O1S = C4S-O2S
 1.4 with sigma of 0.02
 C3S-O2S = C1S-O1S
 2.4 with sigma of 0.02
 C1S-O1S \\sim C3S-O2S
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.7) C2S(0.7) O1S(0.7) C3S(0.3) C4S(0.3) O2S(0.3)
4.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C), C57(H57A,H57B,H57C), C67(H67A,H67B,H67C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C6(H6A), C7(H7A), C8(H8A), C12(H12A), C13(H13A),
 C15(H15A), C16(H16A), C22(H22A), C23(H23A), C25(H25A), C26(H26A), C32(H32A),
 C33(H33A), C35(H35A), C36(H36A), C42(H42A), C43(H43A), C45(H45A), C46(H46A),
 C52(H52A), C53(H53A), C55(H55A), C56(H56A), C62(H62A), C63(H63A), C65(H65A),
 C66(H66A)
;
_olex2_submission_special_instructions 'No special instructions were received'