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_7228613
_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         'C48 H55 Mo2 O2 P1 Sn1'
_chemical_formula_sum            'C48 H55 Mo2 O2 P Sn'
_chemical_formula_weight         1005.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                78.476(6)
_cell_angle_beta                 80.063(6)
_cell_angle_gamma                76.777(6)
_cell_formula_units_Z            4
_cell_length_a                   10.8296(8)
_cell_length_b                   18.5024(12)
_cell_length_c                   24.3014(16)
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9878
_cell_measurement_theta_min      2.8444
_cell_volume                     4603.4(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_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    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1646
_diffrn_reflns_av_unetI/netI     0.2949
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41823
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         70.547
_diffrn_reflns_theta_min         2.853
_exptl_absorpt_coefficient_mu    9.266
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.4962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether and petroleum ether'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         6.008
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         16732
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.2011
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2538
_refine_ls_wR_factor_ref         0.3114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6112
_reflns_number_total             16732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06439j3.cif
_cod_data_source_block           compound4b
_cod_original_formula_sum        'C48 H55 Mo2 O2 P1 Sn1'
_cod_database_code               7228613
_shelxl_version_number           2014-3
_shelx_res_checksum              9314