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_7702974
_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         '2(C38 H66 Br3 Ce Ir2 N4 P2)'
_chemical_formula_sum            'C76 H130 Br6 Ce2 Ir4 N8 P4'
_chemical_formula_weight         2808.25
_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                91.439(2)
_cell_angle_beta                 104.9590(10)
_cell_angle_gamma                109.7390(10)
_cell_formula_units_Z            2
_cell_length_a                   14.3632(5)
_cell_length_b                   19.3199(7)
_cell_length_c                   21.3343(7)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    193
_cell_measurement_theta_max      53.80
_cell_measurement_theta_min      3.03
_cell_volume                     5342.3(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.991
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74998
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.847
_diffrn_reflns_theta_min         1.879
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.149
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.3984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.5308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.651
_refine_diff_density_min         -3.818
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         19372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0895P)^2^+30.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16487
_reflns_number_total             19372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04555d2.cif
_cod_data_source_block           1_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7702971--7702974.cif.'
_cod_database_code               7702974
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.353
_shelx_estimated_absorpt_t_min   0.178
_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:
 C69(H69), C32(H32), C36(H36), C31(H31), C49(H49), C70(H70), C17(H17),
 C55(H55), C73(H73), C35(H35), C14(H14), C28(H28), C24(H24), C20(H20), C27(H27),
  C68(H68), C74(H74), C58(H58), C23(H23), C52(H52), C61(H61), C64(H64),
 C65(H65), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C5(H5A,H5B), C43(H43A,H43B), C42(H42A,H42B), C1(H1A,H1B),
 C3(H3A,H3B), C40(H40A,H40B), C39(H39A,H39B), C76(H76A,H76B), C4(H4A,H4B),
 C2(H2A,H2B), C34(H34A,H34B), C38(H38A,H38B), C37(H37A,H37B), C33(H33A,H33B),
 C75(H75A,H75B), C25(H25A,H25B), C66(H66A,H66B), C63(H63A,H63B), C30(H30A,H30B),
  C29(H29A,H29B), C67(H67A,H67B), C72(H72A,H72B), C71(H71A,H71B), C62(H62A,
 H62B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C48(H48), C45(H45), C47(H47), C8(H8), C46(H46), C9(H9)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C57(H57A,H57B,H57C), C53(H53A,H53B,
 H53C), C21(H21A,H21B,H21C), C60(H60A,H60B,H60C), C54(H54A,H54B,H54C), C50(H50A,
 H50B,H50C), C22(H22A,H22B,H22C), C56(H56A,H56B,H56C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C59(H59A,H59B,H59C), C16(H16A,H16B,
 H16C), C51(H51A,H51B,H51C)
;
_olex2_submission_special_instructions 'No special instructions were received'