Lanthanide mixed-ligand complexes of the [Ln(CAPh)3(Phen)] and [LaxEu1-x(CAPh)3(Phen)] (CAPh = carbacylamidophosphate) type. A comparative study of their spectral properties.
Litsis, Olena O.; Ovchynnikov, Vladimir A.; Scherbatskii, Vasyl P.; Nedilko, Sergiy G.; Sliva, Tatiana Yu; Dyakonenko, Viktoriya V.; Shishkin, Oleg V.; Davydov, Valentine I.; Gawryszewska, Paula; Amirkhanov, Vladimir M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15508–15522; doi:10.1039/c5dt02557e

data_7035945
_publ_section_title
;
 Lanthanide mixed-ligand complexes of the [Ln(CAPh)3(Phen)] and
 [LaxEu1-x(CAPh)3(Phen)] (CAPh = carbacylamidophosphate) type. A
 comparative study of their spectral properties.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15508
_journal_page_last               15522
_journal_paper_doi               10.1039/c5dt02557e
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C48 H68 Cl9 N11 O6 P3 Tb'
_chemical_formula_sum            'C48 H68 Cl9 N11 O6 P3 Tb'
_chemical_formula_weight         1466.01
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-09-30 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2035(5)
_cell_length_b                   14.6551(2)
_cell_length_c                   17.4656(4)
_cell_measurement_reflns_used    13774
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9730
_cell_measurement_theta_min      3.1110
_cell_volume                     6451.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   67.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993   57.0000   30.0000 26

  2 omega   -3.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993   77.0000  120.0000 100

  3 omega   -5.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993   82.0000 -132.0000 41

  4 omega  -25.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993  -99.0000    0.0000 92

  5 omega  -42.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993    0.0000  -30.0000 119

  6 omega  -19.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6993  -57.0000 -120.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0237408000
_diffrn_orient_matrix_UB_12      -0.0167338000
_diffrn_orient_matrix_UB_13      -0.0167046000
_diffrn_orient_matrix_UB_21      0.0057849000
_diffrn_orient_matrix_UB_22      -0.0442742000
_diffrn_orient_matrix_UB_23      0.0141291000
_diffrn_orient_matrix_UB_31      -0.0139535000
_diffrn_orient_matrix_UB_32      0.0101144000
_diffrn_orient_matrix_UB_33      0.0342205000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55253
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         14018
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+1.0504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                11141
_reflns_number_total             14018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02557e2.cif
_cod_data_source_block           kiev210
_cod_depositor_comments
'Adding full bibliography for 7035945--7035947.cif.'
_cod_database_code               7035945
_reflns_odcompleteness_completeness 92.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.37
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2A-C14
 1.75 with sigma of 0.005
 Cl3A-C14
 1.75 with sigma of 0.005
 Cl3B-C14
 1.75 with sigma of 0.005
 Cl1A-C14
 1.75 with sigma of 0.005
 Cl1B-C14
 1.75 with sigma of 0.005
 Cl2B-C14
 1.75 with sigma of 0.005
3. Others
 Fixed Sof: Cl2A(0.5) Cl3A(0.75) Cl2B(0.5) Cl3B(0.25) Cl1B(0.5) Cl1A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'