Sn‒H bond additions to asymmetric trigonal phosphinidene-bridged dimolybdenum complexes
Alvarez, M. Angeles; Amor, Inmaculada; García, M. Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Suárez, Jaime; RSC Adv. 7 (2017) 33293–; doi:10.1039/C7RA06439J

data_7228614
_publ_section_title
;
 Sn--H bond additions to asymmetric trigonal phosphinidene-bridged
 dimolybdenum complexes
;
_journal_issue                   53
_journal_name_full               'RSC Adv.'
_journal_page_first              33293
_journal_paper_doi               10.1039/C7RA06439J
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C31 H43 Mo2 O2 P1'
_chemical_formula_sum            'C31 H43 Mo2 O2 P'
_chemical_formula_weight         670.50
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.2480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3155(3)
_cell_length_b                   16.7360(4)
_cell_length_c                   15.9369(6)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      1.018
_cell_volume                     2946.09(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22174
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.238
_diffrn_reflns_theta_min         1.844
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  1.049
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran and petroleum ether'
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0450
_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^)+(0.1079P)^2^+9.3484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3952
_reflns_number_total             5292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06439j3.cif
_cod_data_source_block           compound3
_cod_original_formula_sum        'C31 H43 Mo2 O2 P1'
_cod_database_code               7228614
_shelxl_version_number           2014-3
_shelx_res_checksum              10418