X-ray crystallographic, luminescence and NMR studies of phenacyldiphenylphosphine oxide with the Ln(iii) ions Sm, Eu, Gd, Tb and Dy
G. Leach, Erin; Shady, Justin R.; Boyden, Adam C.; Emig, Anne-lise; Henry, Alyssa T.; Connor, Emily K.; Staples, Richard J.; Schaertel, Stephanie; Werner, Eric J.; Biros, Shannon M.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02678A

data_7044597
_publ_section_title
;
 X-ray crystallographic, luminescence and NMR studies of
 phenacyldiphenylphosphine oxide with the Ln(iii) ions Sm, Eu, Gd, Tb and
 Dy
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02678A
_journal_year                    2017
_chemical_formula_moiety         'C40 H34 Eu N3 O13 P2, 2(C H Cl3)'
_chemical_formula_sum            'C42 H36 Cl6 Eu N3 O13 P2'
_chemical_formula_weight         1217.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-10 deposited with the CCDC.
2017-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                71.5480(10)
_cell_angle_beta                 80.1730(10)
_cell_angle_gamma                72.0490(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5305(12)
_cell_length_b                   14.0929(14)
_cell_length_c                   16.2116(16)
_cell_measurement_reflns_used    6295
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      19.666
_cell_measurement_theta_min      2.252
_cell_volume                     2575.0(4)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1507
_diffrn_reflns_av_unetI/netI     0.1278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51489
_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         25.739
_diffrn_reflns_theta_min         1.329
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0821 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.9251. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1216
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'slow diffusion of hexane into a solution of chloroform'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.862
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9820
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0763P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6004
_reflns_number_total             9820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02678a2.cif
_cod_data_source_block           gvs414b
_cod_database_code               7044597
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 Cl1X, Cl2X, Cl3X, C1X
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Cl1Y, Cl2Y, Cl3Y, C1Y
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Cl1X \\sim Cl2X \\sim Cl3X \\sim C1X: within 1.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Cl1Y \\sim Cl2Y \\sim Cl3Y \\sim C1Y: within 1.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Same fragment restrains
{Cl1S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl1X, C1X}
{Cl1S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl1Y, C1Y}
5. Others
 Fixed Sof: Cl1X(0.5) C1X(0.5) H1X(0.5) Cl2X(0.5) Cl3X(0.5) Cl1Y(0.5) C1Y(0.5)
 H1Y(0.5) Cl2Y(0.5) Cl3Y(0.5)
6.a Ternary CH refined with riding coordinates:
 C1X(H1X), C1Y(H1Y), C1S(H1S)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C4A(H4A),
  C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A),
 C20A(H20A)
;
_olex2_submission_special_instructions 'No special instructions were received'