Reactions of cerium complexes with transition metal nitrides: synthesis and structure of heterometallic cerium complexes containing bridging catecholate ligands.
Cheung, Wai-Man; Au-Yeung, Ka-Chun; Wong, Kai-Hong; So, Yat-Ming; Sung, Herman H. Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13458–13465; doi:10.1039/c9dt02959a

data_7700874
_publ_section_title
;
 Reactions of cerium complexes with transition metal nitrides: synthesis
 and structure of heterometallic cerium complexes containing bridging
 catecholate ligands.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13458
_journal_page_last               13465
_journal_paper_doi               10.1039/c9dt02959a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C53 H111 Ce Cl2 Co3 N O29 P9 Ru'
_chemical_formula_sum            'C53 H111 Ce Cl2 Co3 N O29 P9 Ru'
_chemical_formula_weight         1994.03
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-12 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                114.874(4)
_cell_angle_beta                 92.656(3)
_cell_angle_gamma                103.883(3)
_cell_formula_units_Z            2
_cell_length_a                   15.0838(5)
_cell_length_b                   17.4193(7)
_cell_length_c                   17.9226(7)
_cell_measurement_reflns_used    10612
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.7940
_cell_measurement_theta_min      4.8230
_cell_volume                     4089.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   44.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -30.0000 47

  2 omega  -48.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  -60.0000 80

  3 omega  -49.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  150.0000 84

  4 omega  -95.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  125.0000  150.0000 93

  5 omega -114.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000    0.0000 103

  6 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000  -60.0000 96

  7 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000   30.0000 98

  8 omega   55.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000   60.0000 60

  9 omega   41.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000   90.0000 50

 10 omega   33.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  120.0000 58

 11 omega   33.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   30.0000 51

 12 omega   34.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  150.0000 74

 13 omega   42.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -120.0000 49

 14 omega   32.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000 -120.0000 109
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0958655000
_diffrn_orient_matrix_UB_12      0.0057669000
_diffrn_orient_matrix_UB_13      0.0392900000
_diffrn_orient_matrix_UB_21      0.0173348000
_diffrn_orient_matrix_UB_22      0.0997941000
_diffrn_orient_matrix_UB_23      0.0544086000
_diffrn_orient_matrix_UB_31      -0.0435452000
_diffrn_orient_matrix_UB_32      -0.0189488000
_diffrn_orient_matrix_UB_33      0.0687817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23782
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.490
_diffrn_reflns_theta_min         4.451
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         14549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12198
_reflns_number_total             14549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02959a2.cif
_cod_data_source_block           ka56cult
_cod_depositor_comments
'Adding full bibliography for 7700874--7700876.cif.'
_cod_database_code               7700874
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cp3 Co3 Et18 O27 Ce1 Ru N Cl2 '
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.557
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O20(H20A,H20B)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B),
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C61(H61A,H61B), C63(H63A,H63B),
  C65(H65A,H65B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C10(H10), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20C,H20D,H20E), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C72(H72A,
 H72B,H72C)
;
_shelx_res_checksum              56188
_olex2_submission_special_instructions 'No special instructions were received'