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_4348152
_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 O14 S2, 1.6(C H2 Cl2), 0.4(C Cl2)'
_chemical_formula_sum            'C104 H102 Cl4 Mo4 N12 O14 S2'
_chemical_formula_weight         2333.66
_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                105.374(3)
_cell_angle_beta                 98.551(3)
_cell_angle_gamma                96.329(3)
_cell_formula_units_Z            1
_cell_length_a                   12.4999(3)
_cell_length_b                   14.1504(5)
_cell_length_c                   15.5088(7)
_cell_measurement_reflns_used    6491
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      62.7400
_cell_measurement_theta_min      3.7300
_cell_volume                     2583.19(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      173.01(10)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -50.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184   57.0000 -120.0000 86

  2 omega -101.00  -75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184  -57.0000   90.0000 26

  3 omega  -32.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184  -77.0000    0.0000 93

  4 omega    4.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   77.0000  120.0000 94

  5 omega   50.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       33.1184  178.0000   30.0000 59

  6 omega   71.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   30.0000 -150.0000 79

  7 omega   19.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -89.0000  -46.1153 79

  8 omega   79.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000  160.7324 27

  9 omega   23.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000   60.0000 49

 10 omega   19.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000  -30.0000 50

 11 omega   33.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000  -90.0000 35

 12 omega   27.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -150.0000 40

 13 omega   35.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -91.0000   26.6249 60

 14 omega   32.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -60.0000 25

 15 omega   18.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000    0.0000 -180.0000 134

 16 omega   19.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000   83.2019 95

 17 omega   20.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -92.0000  160.7324 48

 18 omega   41.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -61.0000  150.0000 65

 19 omega   30.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000 -111.0000  150.0000 31

 20 omega   20.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -180.0000 31

 21 omega   44.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -93.0000  -92.1255 55
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0053571000
_diffrn_orient_matrix_UB_12      -0.1103218000
_diffrn_orient_matrix_UB_13      -0.0509751000
_diffrn_orient_matrix_UB_21      0.0262220000
_diffrn_orient_matrix_UB_22      -0.0235540000
_diffrn_orient_matrix_UB_23      0.0916003000
_diffrn_orient_matrix_UB_31      -0.1233247000
_diffrn_orient_matrix_UB_32      -0.0185775000
_diffrn_orient_matrix_UB_33      0.0017742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15115
_diffrn_reflns_theta_full        62.69
_diffrn_reflns_theta_max         62.69
_diffrn_reflns_theta_min         3.28
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         8157
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+3.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                6762
_reflns_number_total             8157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01021_si_002.cif
_cod_data_source_block           OS-naph-OS
_cod_original_cell_volume        2583.20(16)
_cod_database_code               4348152
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1SA,H1SB} of C1S, {H2SA,H2SB} of C2S, {H4SA,H4SB} of C4S,
   {H5SA,H5SB} of C5S, {H22A,H22B} of C22
 At 1.5 times of:
  All C(H,H,H) groups, {H27A,H27C} of C27
2. Restrained distances
 C1S-Cl1 = C1S-Cl2 = C2S-Cl3 = C2S-Cl4 = C3S-Cl5 = C3S-Cl6 = C4S-Cl7 = C4S-Cl8
 1.78 with sigma of 0.02
 C5S-Cl9 = C5S-Cl10
 1.78 with sigma of 0.02
 Cl1-Cl2 = Cl3-Cl4 = Cl5-Cl6 = Cl7-Cl8 = Cl9-Cl10
 2.78 with sigma of 0.02
 O2-C27 = O2A-C27A
 1.42 with sigma of 0.02
 C24-O2 = C24-O2A
 1.35 with sigma of 0.02
 C24-C27 \\sim C24-C27A
 with sigma of 0.02
3. Others
 Sof(O2A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(O2)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Fixed Sof: Cl1(0.2) C1S(0.2) H1SA(0.2) H1SB(0.2) Cl2(0.2) Cl3(0.2) C2S(0.2)
 H2SA(0.2) H2SB(0.2) Cl4(0.2) Cl5(0.2) C3S(0.2) Cl6(0.2) Cl7(0.2) C4S(0.2)
 H4SA(0.2) H4SB(0.2) Cl8(0.2) Cl9(0.2) C5S(0.2) H5SA(0.2) H5SB(0.2) Cl10(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB)
4.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C37(H37A,H37B,
 H37C), C47(H47A,H47B,H47C), C57(H57A,H57B,H57C), C67(H67A,H67B,H67C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C6(H6A), C7(H7A), C9(H9A), C12(H12A), C13(H13A),
 C15(H15A), C16(H16A), 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'