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_7228612
_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         'C49 H57 Mo2 O2 P1 Sn1'
_chemical_formula_sum            'C49 H57 Mo2 O2 P Sn'
_chemical_formula_weight         1019.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.5640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.26510(10)
_cell_length_b                   22.5628(2)
_cell_length_c                   14.59250(10)
_cell_measurement_reflns_used    11952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7103
_cell_measurement_theta_min      3.0342
_cell_volume                     4353.65(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    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22458
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.809
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85588
_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            red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: deithyl ether and petroleum ethar'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0677P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             8547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06439j3.cif
_cod_data_source_block           compound8b
_cod_original_formula_sum        'C49 H57 Mo2 O2 P1 Sn1'
_cod_database_code               7228612
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2016/6
_shelx_res_checksum              35186