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_7044595
_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 H36 N3 O14 P2 Tb'
_chemical_formula_sum            'C40 H36 N3 O14 P2 Tb'
_chemical_formula_weight         1003.58
_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   mixed
_atom_sites_solution_primary     direct
_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                72.0460(10)
_cell_angle_beta                 75.8340(10)
_cell_angle_gamma                66.6960(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2287(12)
_cell_length_b                   11.6265(12)
_cell_length_c                   18.433(2)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.304
_cell_measurement_theta_min      2.177
_cell_volume                     2081.6(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         1.963
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0657 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8910.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'slow diffusion of hexane into a solution of chloroform'
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0371
_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^)+(0.0285P)^2^+0.5611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6566
_reflns_number_total             7587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02678a2.cif
_cod_data_source_block           gvs813a
_cod_database_code               7044595
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.620
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB)
2.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'