Isolation of heterometallic cerium(iii) complexes with a multidentate nitrogen-phosphorus ligand.
Xin, Xiaoqing; Zhu, Congqing; Dalton transactions (Cambridge, England : 2003) 49 (2020) 603–607; doi:10.1039/c9dt04555d

data_7702972
_publ_section_title
;
 Isolation of heterometallic cerium(iii) complexes with a multidentate
 nitrogen-phosphorus ligand.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              603
_journal_page_last               607
_journal_paper_doi               10.1039/c9dt04555d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43.61 H83.08 Br3 Ce2 Li N8 P4'
_chemical_formula_sum            'C44 H84 Br3 Ce2 Li N8 P4'
_chemical_formula_weight         1375.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-27 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.1430(10)
_cell_angle_beta                 100.1770(10)
_cell_angle_gamma                102.7280(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4128(4)
_cell_length_b                   15.6235(5)
_cell_length_c                   17.6653(5)
_cell_measurement_reflns_used    9151
_cell_measurement_temperature    193
_cell_measurement_theta_max      53.86
_cell_measurement_theta_min      4.39
_cell_volume                     3250.88(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40061
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.919
_diffrn_reflns_theta_min         2.237
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.295
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0692 after correction.
The Ratio of minimum to maximum transmission is 0.5890.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         11631
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0508P)^2^+9.2392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11253
_reflns_number_total             11631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04555d2.cif
_cod_data_source_block           1_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7702971--7702974.cif.'
_cod_original_cell_volume        3250.87(17)
_cod_database_code               7702972
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.258
_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 C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C42) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C36(H36), C33(H33), C42(H42), C21(H21), C24(H24), C39(H39), C27(H27), C30(H30)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C12(H12A,H12B), C11(H11A,H11B), C15(H15A,
 H15B), C1(H1A,H1B), C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C19(H19), C10(H10), C8(H8), C7(H7), C17(H17), C9(H9)
4.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C35(H35A,
 H35B,H35C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C),
 C31(H31A,H31B,H31C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,
 H44C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'