Synthesis and structural, redox and photophysical properties of tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
McPherson, James N.; Abad Galan, Laura; Iranmanesh, Hasti; Massi, Massimiliano; Colbran, Stephen B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9365–9375; doi:10.1039/c9dt01262a

data_7700170
_publ_section_title
;
 Synthesis and structural, redox and photophysical properties of
 tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9365
_journal_page_last               9375
_journal_paper_doi               10.1039/c9dt01262a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C51 H42 N9 O6 Sm, 0.5(H2 O)'
_chemical_formula_sum            'C51 H43 N9 O6.5 Sm'
_chemical_formula_weight         1036.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.85(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.177(3)
_cell_length_b                   13.222(3)
_cell_length_c                   19.402(4)
_cell_measurement_reflns_used    11057
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      1.94
_cell_volume                     4406.0(16)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65218
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       cube
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.023
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0097(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9559
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+8.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8469
_reflns_number_total             9559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01262a2.cif
_cod_data_source_block           james_sm1_a
_cod_depositor_comments
'Adding full bibliography for 7700168--7700170.cif.'
_cod_original_cell_volume        4406.0(15)
_cod_original_formula_sum        'C51 H43 N9 O6.50 Sm'
_cod_database_code               7700170
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2C-C9C
 1.487 with sigma of 0.02
 C9C-O2C
 1.46 with sigma of 0.02
3. Restrained angles
 C8C-O2C-C9C
 fixed at 120 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9C) = Uanis(C9C')
5. Rigid body (RIGU) restrains
 O2C, C8C, C9C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9C', C9C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9C, C9C'
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.04
6. Others
 Fixed Sof: O1C(0.53919) O1C'(0.46081) O2C(0.44916) O2C'(0.55084) C9C(0.55553)
 H9CA(0.55553) H9CB(0.55553) H9CC(0.55553) C9C'(0.44447) H9CD(0.44447)
 H9CE(0.44447) H9CF(0.44447) O1(0.5) H1D(0.5) H1E(0.5)
7.a Free rotating group:
 O1(H1D,H1E)
7.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1C(H1C), C2A(H2A), C2B(H2B), C2C(H2C), C3A(H3A),
 C3B(H3B), C3C(H3C), C4A(H4A), C4B(H4B), C4C(H4C), C14A(H14A), C14B(H14B),
 C14C(H14C), C15A(H15A), C15B(H15B), C15C(H15C), C16A(H16A), C16B(H16B),
 C16C(H16C), C17A(H17A), C17B(H17B), C17C(H17C)
7.c Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC), C9C'(H9CD,H9CE,
 H9CF), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G,H10H,H10I)
;
_olex2_submission_special_instructions 'No special instructions were received'