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_7032072
_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_compound_source        'see text'
_chemical_formula_moiety         'C72 H74 Mo4 N6 O8 P4, 4(B F4), 4(C3 H5 N)'
_chemical_formula_sum            'C84 H94 B4 F16 Mo4 N10 O8 P4'
_chemical_formula_weight         2226.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 116.427(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.183(2)
_cell_length_b                   15.535(2)
_cell_length_c                   18.873(2)
_cell_measurement_reflns_used    9487
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      1.25
_cell_volume                     4774.0(10)
_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  'SHELXL2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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_unetI/netI     0.0298
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8821
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0657P)^2^+5.8818P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                8337
_reflns_number_total             8821
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            c4dt01560f2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7032072--7032073.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7032072