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_7047358
_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         'C43 H71 N4 O6 Sm, C25, H35 N2'
_chemical_formula_sum            'C68 H106 N6 O6 Sm'
_chemical_formula_weight         1253.93
_chemical_name_systematic
;
 [Sm(2,2,2-crypt){CH[N(Dipp)]2}[CH[N(Dipp)]2]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.036(2)
_cell_length_b                   21.134(4)
_cell_length_c                   28.094(6)
_cell_measurement_reflns_used    41792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0870
_cell_measurement_theta_min      3.9740
_cell_volume                     6552(2)
_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-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0517
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            78072
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.284
_diffrn_reflns_theta_min         3.778
_exptl_absorpt_coefficient_mu    7.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73432
_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            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 5657 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0128(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         13630
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+1.6786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                13234
_reflns_number_total             13630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03427c2.cif
_cod_data_source_block           SB610
_cod_depositor_comments
'Adding full bibliography for 7047353--7047362.cif.'
_cod_database_code               7047358
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.414
_shelx_res_checksum              82278