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_7035947
_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_formula_moiety         'C48 H68 Cl9 N11 Nd O6 P3'
_chemical_formula_sum            'C48 H68 Cl9 N11 Nd O6 P3'
_chemical_formula_weight         1451.33
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-06-24 deposited with the CCDC.
2015-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                97.887(4)
_cell_angle_beta                 105.308(4)
_cell_angle_gamma                100.223(4)
_cell_formula_units_Z            4
_cell_length_a                   15.6215(8)
_cell_length_b                   18.3288(9)
_cell_length_c                   22.9355(11)
_cell_measurement_temperature    100(2)
_cell_volume                     6115.1(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51315
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97926
_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    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2956
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         28073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                19626
_reflns_number_total             28073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02557e2.cif
_cod_data_source_block           kiev213lt
_cod_depositor_comments
;
Adding full bibliography for 7035945--7035947.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6115.1(5)
_cod_original_formula_moiety     '2(C48 H68 Cl9 N11 Nd O6 P3)'
_cod_original_formula_sum        'C96 H136 Cl18 N22 Nd2 O12 P6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2902.67
_cod_database_code               7035947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,H18B), C19A(H19A,
 H19B), C20A(H20A,H20B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B),
 C24A(H24A,H24B), C27A(H27A,H27B), C28A(H28A,H28B), C29A(H29A,H29B), C30A(H30A,
 H30B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B),
 C35A(H35A,H35B), C36A(H36A,H36B), C39A(H39A,H39B), C40A(H40A,H40B), C41A(H41A,
 H41B), C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,H44B), C45A(H45A,H45B),
 C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B), C15B(H15C,H15D), C16B(H16C,
 H16D), C17B(H17C,H17D), C18B(H18C,H18D), C19B(H19C,H19D), C20B(H20C,H20D),
 C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D), C24B(H24C,H24D), C27B(H27C,
 H27D), C28B(H28C,H28D), C29B(H29C,H29D), C30B(H30C,H30D), C31B(H31C,H31D),
 C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D), C35B(H35C,H35D), C36B(H36C,
 H36D), C39B(H39C,H39D), C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D),
 C43B(H43C,H43D), C44B(H44C,H44D), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,
 H47D), C48B(H48C,H48D)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C6A(H6A), C7A(H7A), C10A(H10A), C11A(H11A),
 C12A(H12A), C1B(H1B), C2B(H2B), C3B(H3B), C6B(H6B), C7B(H7B), C10B(H10B),
 C11B(H11B), C12B(H12B)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'