Phosphoryl-Ligand Adducts of Rare Earth-TriNOx Complexes: Systematic Studies and Implications for Separations Chemistry
Cheisson, Thibault; Cole, Bren E.; Manor, Brian C.; Carroll, Patrick J.; Schelter, Eric J.; ACS Sustainable Chemistry & Engineering 7 (2019) 4993–; doi:10.1021/acssuschemeng.8b05638

data_4515211
_publ_section_title
;
 Phosphoryl-Ligand Adducts of Rare Earth-TriNOx Complexes: Systematic
 Studies and Implications for Separations Chemistry
;
_journal_issue                   5
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_page_first              4993
_journal_paper_doi               10.1021/acssuschemeng.8b05638
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C39 H60 N4 Nd O4 P'
_chemical_formula_sum            'C39 H60 N4 Nd O4 P'
_chemical_formula_weight         824.12
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4859(5)
_cell_length_b                   17.8257(5)
_cell_length_c                   27.8903(8)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.47
_cell_volume                     8190.2(4)
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            123560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         1.461
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       prism
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
TITL mo_40046a_0m_a.res in C2/c
CELL   16.4859   17.8257   27.8903     90.00     92.19     90.00
SPGR C2/c
C101 0.967 0.279 0.205 !      17.38 eA-3
C102 0.988 0.347 0.256 !       4.50 eA-3
Q103 0.893 0.326 0.454 !       2.40 eA-3
C104 0.030 0.219 0.236 !       1.98 eA-3
C105 0.973 0.310 0.297 !       1.18 eA-3
Q106 0.096 0.216 0.062 !       1.04 eA-3
Q107 0.823 0.299 0.485 !       0.92 eA-3
Q108 0.966 0.392 0.485 !       0.83 eA-3
Q109 0.780 0.462 0.397 !       0.83 eA-3
Q110 0.705 0.346 0.375 !       0.82 eA-3
Q111 0.982 0.452 0.021 !       0.80 eA-3
Q112 0.670 0.379 0.330 !       0.80 eA-3
Q113 0.886 0.453 0.329 !       0.77 eA-3
Q114 0.801 0.502 0.451 !       0.75 eA-3
Q115 0.279 0.985 0.363 !       0.75 eA-3
Q116 0.779 0.485 0.363 !       0.75 eA-3
Q117 0.642 0.209 0.456 !       0.74 eA-3
Q118 0.238 0.278 0.432 !       0.74 eA-3
Q119 0.194 0.045 0.220 !       0.72 eA-3
Q120 0.641 0.034 0.181 !       0.70 eA-3
C121 0.904 0.283 0.189 !       0.67 eA-3
Q122 0.225 0.029 0.446 !       0.66 eA-3
Q123 0.107 0.020 0.297 !       0.66 eA-3
Q124 0.680 0.330 0.304 !       0.65 eA-3
Q125 0.540 0.406 0.118 !       0.65 eA-3
Q126 0.588 0.386 0.344 !       0.64 eA-3
Q127 0.718 0.420 0.424 !       0.63 eA-3
Q128 0.855 0.344 0.412 !       0.63 eA-3
C129 0.926 0.233 0.198 !       0.59 eA-3
C130 0.074 0.235 0.308 !       0.59 eA-3
Q131 0.075 0.187 0.105 !       0.58 eA-3
Q132 0.294 0.152 0.467 !       0.58 eA-3
Q133 0.555 0.468 0.326 !       0.58 eA-3
Q134 0.253 0.076 0.268 !       0.57 eA-3
Q135 0.669 0.157 0.095 !       0.57 eA-3
Q136 0.676 0.048 0.225 !       0.55 eA-3
Q137 0.535 0.359 0.126 !       0.55 eA-3
Q138 0.460 0.066 0.386 !       0.54 eA-3
Q139 0.857 0.496 0.234 !       0.54 eA-3
Q140 0.707 0.312 0.274 !       0.54 eA-3
Q141 0.236 0.190 0.374 !       0.53 eA-3
Q142 0.513 0.488 0.151 !       0.53 eA-3
Q143 0.529 0.107 0.147 !       0.53 eA-3
Q144 0.285 0.488 0.460 !       0.53 eA-3
Q145 0.355 0.357 0.255 !       0.53 eA-3
Q146 1.003 0.360 0.471 !       0.52 eA-3
Q147 0.535 0.341 0.367 !       0.51 eA-3
Q148 0.329 0.454 0.060 !       0.51 eA-3
Q149 0.185 0.137 0.408 !       0.51 eA-3
;
_refine_diff_density_max         1.834
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+38.9399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                8846
_reflns_number_total             9445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sc8b05638_si_002.cif
_cod_data_source_block           40046
_cod_database_code               4515211
_platon_squeeze_void_probe_radius 1.20