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_4348151
_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 O16, 2(C1 Cl2)'
_chemical_formula_sum            'C104 H100 Cl4 Mo4 N12 O16'
_chemical_formula_weight         2299.52
_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             2015-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                83.485(3)
_cell_angle_beta                 84.650(3)
_cell_angle_gamma                86.793(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0793(4)
_cell_length_b                   13.5740(5)
_cell_length_c                   15.0188(6)
_cell_measurement_reflns_used    7062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.5090
_cell_measurement_theta_min      2.9760
_cell_volume                     2433.42(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2417
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega  -25.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375   57.0000   30.0000 63

  2 omega  -54.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375  -38.0000 -150.0000 76

  3 omega    7.00  162.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431    0.0000   30.0000 155

  4 omega   70.00  110.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431  -77.0000   60.0000 40

  5 omega   69.00  108.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431  -94.0000    0.0000 39

  6 omega   31.00  119.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431 -125.0000 -120.0000 88

  7 omega   37.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375 -179.0000 -120.0000 43

  8 omega   21.00   50.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431  -94.0000    0.0000 29

  9 omega   21.00   48.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431  -77.0000   60.0000 27

 10 omega   16.00  117.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431  -77.0000 -120.0000 101

 11 omega   60.00  146.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -       86.6431   61.0000   30.0000 86

 12 omega  -63.00  -15.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -      -88.5181   30.0000  -30.0000 48

 13 omega  -67.00  -16.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -      -88.5181   77.0000   90.0000 51

 14 omega -116.00  -90.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -      -88.5181   77.0000   90.0000 26

 15 omega  -65.00  -19.00   1.0000    4.7450
omega____ theta____ kappa____ phi______ frames
    -      -88.5181   45.0000 -180.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0633458000
_diffrn_orient_matrix_UB_12      -0.0498356000
_diffrn_orient_matrix_UB_13      -0.0658879000
_diffrn_orient_matrix_UB_21      0.0382551000
_diffrn_orient_matrix_UB_22      0.0793461000
_diffrn_orient_matrix_UB_23      -0.0766306000
_diffrn_orient_matrix_UB_31      0.1047226000
_diffrn_orient_matrix_UB_32      -0.0655510000
_diffrn_orient_matrix_UB_33      -0.0229775000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15542
_diffrn_reflns_theta_full        65.96
_diffrn_reflns_theta_max         65.96
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         8224
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+5.9458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                6232
_reflns_number_total             8224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01021_si_002.cif
_cod_data_source_block           O2-naph-O2
_cod_database_code               4348151
_reflns_odcompleteness_completeness 99.88
_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
 O5-C57 = O5A-C57A
 1.42 with sigma of 0.02
 C54-O5 = C54A-O5A
 1.35 with sigma of 0.02
 C1S-Cl1 = C2S-Cl2
 1.78 with sigma of 0.02
 C2S-Cl3 = C2S-Cl4
 1.78 with sigma of 0.02
 Cl1-Cl2 = Cl3-Cl4
 2.78 with sigma of 0.02
 C54-C57 \\sim C54A-C57A
 with sigma of 0.02
3. Others
 Sof(C51A)=Sof(C52A)=Sof(H52B)=Sof(C53A)=Sof(H53B)=Sof(C54A)=Sof(C55A)=
 Sof(H55B)=Sof(C56A)=Sof(H56B)=Sof(O5A)=Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=
 1-FVAR(1)
 Sof(C51)=Sof(C52)=Sof(H52A)=Sof(C53)=Sof(H53A)=Sof(C54)=Sof(C55)=Sof(H55A)=
 Sof(C56)=Sof(H56A)=Sof(O5)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(1)
 Fixed Sof: Cl1(0.7) C1S(0.7) Cl2(0.7) Cl3(0.3) C2S(0.3) Cl4(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), C57A(H57D,H57E,H57F), 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), C52A(H52B), C53A(H53B), C55A(H55B),
  C56A(H56B), C62(H62A), C63(H63A), C65(H65A), C66(H66A)
4.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56), C51A(C52A,C53A,C54A,C55A,C56A)
;
_olex2_submission_special_instructions 'No special instructions were received'