Loop shaped dicarboxylate-bridged dimolybdenum(ii) bisphosphine compounds - a rational synthesis.
Höhne, Dominik; Herdtweck, Eberhardt; Pöthig, Alexander; Kühn, Fritz E; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15367–15374; doi:10.1039/c4dt01560f

data_7032073
_publ_section_title
;
 Loop shaped dicarboxylate-bridged dimolybdenum(ii) bisphosphine compounds
 - a rational synthesis.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15367
_journal_page_last               15374
_journal_paper_doi               10.1039/c4dt01560f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C76 H80 Mo4 N4 O8 P4, 4(B F4), 6(C3 H5 N)'
_chemical_formula_sum            'C94 H110 B4 F16 Mo4 N10 O8 P4'
_chemical_formula_weight         2362.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                74.092(2)
_cell_angle_beta                 88.172(2)
_cell_angle_gamma                81.785(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4049(5)
_cell_length_b                   18.0187(7)
_cell_length_c                   24.6268(10)
_cell_measurement_reflns_used    9004
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      0.86
_cell_volume                     5239.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2010)'
_computing_publication_material  'PLATON (Spek, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            92300
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.074
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         19171
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0466P)^2^+27.3733P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                15070
_reflns_number_total             19171
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            c4dt01560f2.cif
_cod_data_source_block           hoep_fine
_cod_depositor_comments
'Adding full bibliography for 7032072--7032073.cif.'
_cod_database_code               7032073