1,2,4-Diazaphospholide complexes of yttrium(iii), dysprosium(iii), erbium(iii), and europium(ii,iii): synthesis, X-ray structural characterization, and EPR analysis.
Wang, Yongli; Guo, Wenzhen; Liu, Dongling; Yang, Ying; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 899–903; doi:10.1039/c5dt04285b

data_7037622
_publ_section_title
;
 1,2,4-Diazaphospholide complexes of yttrium(iii), dysprosium(iii),
 erbium(iii), and europium(ii,iii): synthesis, X-ray structural
 characterization, and EPR analysis.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              899
_journal_page_last               903
_journal_paper_doi               10.1039/c5dt04285b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C38 H70 Dy N6 O2 P3'
_chemical_formula_sum            'C38 H70 Dy N6 O2 P3'
_chemical_formula_weight         898.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-12-02 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.531(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5609(6)
_cell_length_b                   12.7972(4)
_cell_length_c                   20.0361(6)
_cell_measurement_reflns_used    3625
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.208
_cell_measurement_theta_min      3.662
_cell_volume                     4645.8(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10733
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.025
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0341P)^2^+1.4107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4130
_reflns_number_total             4560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04285b2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7037620--7037625.cif.'
_cod_database_code               7037622
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: C13(0.6) H13A(0.6) H13B(0.6) H13C(0.6) C14(0.6) H14A(0.6)
 H14B(0.6) H14C(0.6) C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6) C13'(0.4) H13D(0.4)
 H13E(0.4) H13F(0.4) C14'(0.4) H14D(0.4) H14E(0.4) H14F(0.4) C15'(0.4)
 H15D(0.4) H15E(0.4) H15F(0.4) C17(0.5) H17A(0.5) H17B(0.5) C18(0.6) H18A(0.6)
 H18B(0.6) C17'(0.5) H17C(0.5) H17D(0.5) C18'(0.4) H18C(0.4) H18D(0.4)
 Fixed U12: Dy1(0) P2(-0)
 Fixed U23: Dy1(0) P2(0)
 Fixed Uiso: H4A(0.115) H4B(0.115) H4C(0.115) H5A(0.129) H5B(0.129) H5C(0.129)
 H6A(0.123) H6B(0.123) H6C(0.123) H8A(0.198) H8B(0.198) H8C(0.198) H9A(0.224)
 H9B(0.224) H9C(0.224) H10A(0.169) H10B(0.169) H10C(0.169) H13A(0.183)
 H13B(0.183) H13C(0.183) H14A(0.183) H14B(0.183) H14C(0.183) H15A(0.146)
 H15B(0.146) H15C(0.146) H13D(0.178) H13E(0.178) H13F(0.178) H14D(0.156)
 H14E(0.156) H14F(0.156) H15D(0.16) H15E(0.16) H15F(0.16) H16A(0.084)
 H16B(0.084) H17A(0.095) H17B(0.095) H18A(0.09) H18B(0.09) H17C(0.089)
 H17D(0.089) H18C(0.093) H18D(0.093) H19A(0.09) H19B(0.09)
 Fixed X: Dy1(0.5) P2(0.5) H4A(0.3966) H4B(0.3368) H4C(0.3922) H5A(0.4326)
 H5B(0.4596) H5C(0.3761) H6A(0.5321) H6B(0.5522) H6C(0.5255) H8A(0.4689)
 H8B(0.4356) H8C(0.4098) H9A(0.2867) H9B(0.3268) H9C(0.267) H10A(0.3152)
 H10B(0.2927) H10C(0.37) H13A(0.3488) H13B(0.4332) H13C(0.3998) H14A(0.3322)
 H14B(0.3909) H14C(0.311) H15A(0.277) H15B(0.3336) H15C(0.2916) H13D(0.3432)
 H13E(0.4041) H13F(0.4252) H14D(0.2724) H14E(0.316) H14F(0.3435) H15D(0.3522)
 H15E(0.3318) H15F(0.281) H16A(0.6072) H16B(0.5872) H17A(0.6946) H17B(0.7211)
 H18A(0.7824) H18B(0.7492) H17C(0.7084) H17D(0.7054) H18C(0.7817) H18D(0.747)
 H19A(0.6798) H19B(0.6887)
 Fixed Y: H4A(0.7412) H4B(0.6611) H4C(0.6299) H5A(0.7587) H5B(0.661)
 H5C(0.672) H6A(0.603) H6B(0.6312) H6C(0.7188) H8A(0.1743) H8B(0.1279)
 H8C(0.0852) H9A(0.1271) H9B(0.1911) H9C(0.245) H10A(0.162) H10B(0.2789)
 H10C(0.252) H13A(0.0406) H13B(0.0219) H13C(0.1341) H14A(-0.098) H14B(-0.1159)
 H14C(-0.079) H15A(0.1058) H15B(0.1802) H15C(0.0949) H13D(-0.0551) H13E(-
 0.1059) H13F(-0.0167) H14D(-0.0382) H14E(0.0213) H14F(-0.0882) H15D(0.1665)
 H15E(0.1725) H15F(0.1105) H16A(0.3192) H16B(0.4409) H17A(0.5162) H17B(0.4215)
 H18A(0.4304) H18B(0.3191) H17C(0.306) H17D(0.4178) H18C(0.3845) H18D(0.4954)
 H19A(0.4754) H19B(0.3392)
 Fixed Z: Dy1(0.25) P2(0.25) H4A(0.2922) H4B(0.3044) H4C(0.2589) H5A(0.4189)
 H5B(0.4647) H5C(0.4287) H6A(0.3221) H6B(0.4001) H6C(0.3456) H8A(0.4404)
 H8B(0.3678) H8C(0.4321) H9A(0.3477) H9B(0.2997) H9C(0.3326) H10A(0.4717)
 H10B(0.4555) H10C(0.5018) H13A(0.0438) H13B(0.0732) H13C(0.0749) H14A(0.1841)
 H14B(0.1395) H14C(0.105) H15A(0.1156) H15B(0.1623) H15C(0.1954) H13D(0.0736)
 H13E(0.131) H13F(0.0851) H14D(0.1771) H14E(0.2417) H14F(0.2226) H15D(0.1024)
 H15E(0.1742) H15F(0.1145) H16A(0.4173) H16B(0.413) H17A(0.422) H17B(0.4722)
 H18A(0.3704) H18B(0.3816) H17C(0.4466) H17D(0.4791) H18C(0.3899) H18D(0.3972)
 H19A(0.2972) H19B(0.2786)
;
_shelx_res_checksum              8960