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_7702971
_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         'C44 H83 Br3 Ce2 Li2 N8 P4'
_chemical_formula_sum            'C44 H83 Br3 Ce2 Li2 N8 P4'
_chemical_formula_weight         1381.91
_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                70.3330(10)
_cell_angle_beta                 81.1600(10)
_cell_angle_gamma                84.0940(10)
_cell_formula_units_Z            2
_cell_length_a                   14.0359(4)
_cell_length_b                   14.1167(4)
_cell_length_c                   17.7636(6)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.26
_cell_volume                     3270.04(17)
_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      173
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24842
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.183
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1338 before and 0.0389 after correction.
The Ratio of minimum to maximum transmission is 0.6514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9886
_reflns_number_total             11417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04555d2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7702971--7702974.cif.'
_cod_database_code               7702971
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.731
_shelx_estimated_absorpt_t_min   0.731
_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.a Ternary CH refined with riding coordinates:
 C42(H42), C30(H30), C39(H39), C27(H27), C24(H24), C21(H21), C33(H33), C36(H36)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C13(H13A,
 H13B), C14(H14A,H14B), C12(H12A,H12B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C17(H17), C7(H7), C20(H20), C9(H9), C8(H8), C18(H18),
 C19(H19)
2.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C26(H26A,
 H26B,H26C), C44(H44A,H44B,H44C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C),
 C41(H41A,H41B,H41C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C), C37(H37A,H37B,
 H37C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'