Different Reductive Reactivities of SmCpx2(THF)n (Cpx = C5Me5 and C5H3tBu2) Samarocenes toward P2Ph4: THF Ring-Opening and Ligand-Exchange Pathways
Pushkarevsky, Nikolay A.; Ilyin, Igor Yu.; Petrov, Pavel A.; Samsonenko, Denis G.; Ryzhikov, Maxim R.; Roesky, Peter W.; Konchenko, Sergey N.; Organometallics 36 (2017) 1287–; doi:10.1021/acs.organomet.7b00014

data_4087334
_publ_section_title
;
 Different Reductive Reactivities of SmCpx2(THF)n (Cpx = C5Me5 and
 C5H3tBu2) Samarocenes toward P2Ph4: THF Ring-Opening and Ligand-Exchange
 Pathways
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1287
_journal_paper_doi               10.1021/acs.organomet.7b00014
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C72 H96 O2 P2 Sm2'
_chemical_formula_weight         1356.12
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
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_cell_angle_gamma                84.906(2)
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_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      3.53
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_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
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_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.819
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_diffrn_reflns_theta_max         29.062
_diffrn_reflns_theta_min         3.406
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0164P)^2^+0.2352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6486
_reflns_number_total             7091
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om7b00014_si_002.cif
_cod_data_source_block           3b
_cod_original_cell_volume        1616.15(10)
_cod_database_code               4087334
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.805
_shelx_res_checksum              47411
_shelx_hkl_checksum              11575