Synthesis and reactivity of rare-earth metal phosphaethynolates.
Bestgen, Sebastian; Chen, Qien; Rees, Nicholas H.; Goicoechea, Jose M.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13016–13024; doi:10.1039/c8dt03427c

data_7047361
_publ_section_title
;
 Synthesis and reactivity of rare-earth metal phosphaethynolates.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13016
_journal_page_last               13024
_journal_paper_doi               10.1039/c8dt03427c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C56 H78 N4 O3 P2 Sm, C20 H40 Na O8, 0.35(C6 H14), 0.65(C4 H8 O)'
_chemical_formula_sum            'C80.7 H128.1 N4 Na O11.65 P2 Sm'
_chemical_formula_weight         1576.04
_chemical_name_systematic
;
 [Na(18-crown-6)(THF)2][Sm(OCP)2{CH[N(Dipp)]2}2(THF)]*0.65THF*0.35hex
;
_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-2013
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.674(3)
_cell_length_b                   24.610(5)
_cell_length_c                   20.762(4)
_cell_measurement_reflns_used    17216
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1290
_cell_measurement_theta_min      3.5690
_cell_volume                     8509(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50089
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.176
_diffrn_reflns_theta_min         3.592
_exptl_absorpt_coefficient_mu    6.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             3346
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.062
_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     972
_refine_ls_number_reflns         17563
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.6786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14545
_reflns_number_total             17563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03427c2.cif
_cod_data_source_block           SB594B
_cod_depositor_comments
'Adding full bibliography for 7047353--7047362.cif.'
_cod_original_formula_sum        'C80.70 H128.10 N4 Na O11.65 P2 Sm'
_cod_database_code               7047361
_shelx_estimated_absorpt_t_min   0.378
_shelx_estimated_absorpt_t_max   0.644
_shelxl_version_number           2013-4
_shelx_res_checksum              29251