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_7700876
_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         'C12 H8 O6 Re, C34 H69 Ce Co2 O20 P6'
_chemical_formula_sum            'C46 H82 Ce Co2 O26 P6 Re'
_chemical_formula_weight         1681.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-15
_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                90
_cell_angle_beta                 99.3323(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.86004(14)
_cell_length_b                   22.5385(3)
_cell_length_c                   24.0165(2)
_cell_measurement_reflns_used    14723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.4800
_cell_measurement_theta_min      3.9150
_cell_volume                     6334.82(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     31.00 108.00   1.00    3.00    --  110.57 -94.00   0.00   77
  2  \w    -70.00  33.00   1.00    2.00    --  -40.57  57.00-120.00  103
  3  \w    -70.00  33.00   1.00    2.00    --  -40.57  77.00  90.00  103
  4  \w    -68.00  35.00   1.00    2.00    --  -40.57  77.00 -30.00  103
  5  \w     43.00 141.00   1.00    3.00    --  110.57 -30.00 -60.00   98
  6  \w     80.00 177.00   1.00    3.00    --  110.57  30.00-180.00   97
  7  \w    100.00 178.00   1.00    3.00    --  110.57 111.00  60.00   78
  8  \w     89.00 170.00   1.00    3.00    --  110.57  45.00 120.00   81
  9  \w     43.00 115.00   1.00    3.00    --  110.57-111.00 -90.00   72
 10  \w     32.00 134.00   1.00    3.00    --  110.57 -77.00  90.00  102
 11  \w     39.00 141.00   1.00    3.00    --  110.57 -30.00 120.00  102
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0443684000
_diffrn_orient_matrix_UB_12      0.0627248000
_diffrn_orient_matrix_UB_13      -0.0100458000
_diffrn_orient_matrix_UB_21      -0.0474326000
_diffrn_orient_matrix_UB_22      -0.0056148000
_diffrn_orient_matrix_UB_23      -0.0634569000
_diffrn_orient_matrix_UB_31      -0.1144175000
_diffrn_orient_matrix_UB_32      0.0265007000
_diffrn_orient_matrix_UB_33      0.0102925000
_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     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35347
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.497
_diffrn_reflns_theta_min         3.730
_diffrn_source                   'micro-focus 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    15.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.763
_exptl_crystal_description       plate
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.533
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         11375
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0480P)^2^+8.0360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9814
_reflns_number_total             11375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02959a2.cif
_cod_data_source_block           hong13cult
_cod_depositor_comments
'Adding full bibliography for 7700874--7700876.cif.'
_cod_original_cell_volume        6334.81(12)
_cod_database_code               7700876
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re Co Ce O15 P3 C29 H45 Cl2'
_reflns_odcompleteness_completeness 99.94
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C40A-C39 \\sim C40-C39
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(P5A) \\sim Ueq, Uanis(P4A) \\sim Ueq, Uanis(P6A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.003
Uanis(C11A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
Uanis(O18A) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O19A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.002
Uanis(O12A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(O16A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 P4A, O12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P5A, O14A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: P4(0.8) P4A(0.2) P5(0.8) P5A(0.2) P6(0.8) P6A(0.2) O11(0.8)
 O12A(0.2) O13(0.8) O14A(0.2) O15(0.8) O16A(0.2) O17(0.8) O17A(0.2) O18(0.8)
 O18A(0.2) O19(0.8) O19A(0.2) C11(0.5) H11A(0.5) H11B(0.5) C11A(0.5) H11C(0.5)
 H11D(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C12A(0.5) H12D(0.5) H12E(0.5)
 H12F(0.5) C40(0.58) C40A(0.42)
6.a Rotating group:
 O10(H10A,H10B), O20(H20A,H20B)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11A(H11C,H11D), 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), C41(H41A,H41B)
6.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C54(H54), C55(H55), C56(H56), C63(H63), C64(H64), C65(H65),
 C66(H66), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C10(H10)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20C,H20D,H20E), C22(H22A,H22B,H22C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              84500
_olex2_date_sample_data_collection 2017-08-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.711