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_7047357
_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
'C76 H117 N4 Na Nd O11 P2, 0.5(C4 H8 O), 0.5(C6 H14)'
_chemical_formula_sum            'C81 H128 N4 Na Nd O11.5 P2'
_chemical_formula_weight         1571.04
_chemical_name_systematic
;
 [Na(18-crown-6)](THF)2][Nd(OCP)2{CH[N(Dipp)]2}2]*0.5THF*0.5hex
;
_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-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                 93.0970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6407(2)
_cell_length_b                   24.6511(3)
_cell_length_c                   20.6049(2)
_cell_measurement_reflns_used    23470
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.2840
_cell_measurement_theta_min      3.7240
_cell_volume                     8440.02(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 0.968
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.541
_diffrn_reflns_theta_min         3.586
_exptl_absorpt_coefficient_mu    5.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             3340
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         17600
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+3.7417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15908
_reflns_number_total             17600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03427c2.cif
_cod_data_source_block           SB630
_cod_depositor_comments
'Adding full bibliography for 7047353--7047362.cif.'
_cod_original_formula_sum        'C81 H128 N4 Na Nd O11.50 P2'
_cod_database_code               7047357
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.374
_shelx_estimated_absorpt_t_max   0.635
_shelx_res_checksum              54216