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_7700875
_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         'C46 H78 Ce Co2 N O22 P6 Ru'
_chemical_formula_sum            'C46 H78 Ce Co2 N O22 P6 Ru'
_chemical_formula_weight         1541.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-05-08
_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                 93.4905(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.9360(3)
_cell_length_b                   13.2047(2)
_cell_length_c                   40.2851(7)
_cell_measurement_reflns_used    8673
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.1710
_cell_measurement_theta_min      3.8560
_cell_volume                     12178.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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     32.00 112.25   0.75    4.00    --  110.57-111.00  90.00  107
  2  \w   -117.00  -7.50   0.75    2.00    --  -40.20 -77.00 120.00  146
  3  \w    -65.00  29.50   0.75    2.00    --  -40.20  37.00 -90.00  126
  4  \w     31.00  97.75   0.75    2.00    --   40.20-125.00 -30.00   89
  5  \w    -34.00  70.25   0.75    2.00    --   40.20 -57.00 -30.00  139
  6  \w     32.00 144.50   0.75    4.00    --  110.57 -77.00 120.00  150
  7  \w     80.00 174.50   0.75    4.00    --  110.57  61.00-120.00  126
  8  \w     36.00 141.00   0.75    4.00    --  110.57 -30.00-150.00  140
  9  \w     61.00 133.75   0.75    4.00    --  110.57 -45.00 -90.00   97
 10  \w     45.00 112.50   0.75    4.00    --  110.57-111.00 -30.00   90
 11  \w     34.00 166.75   0.75    4.00    --  110.57 -15.00  60.00  177
;
_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      -0.0656713000
_diffrn_orient_matrix_UB_12      0.0247788000
_diffrn_orient_matrix_UB_13      0.0005067000
_diffrn_orient_matrix_UB_21      -0.0101028000
_diffrn_orient_matrix_UB_22      -0.0437632000
_diffrn_orient_matrix_UB_23      -0.0353098000
_diffrn_orient_matrix_UB_31      -0.0112222000
_diffrn_orient_matrix_UB_32      -0.1051660000
_diffrn_orient_matrix_UB_33      0.0148082000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            33582
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             6264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.152
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         10936
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0600P)^2^+119.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9065
_reflns_number_total             10936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02959a2.cif
_cod_data_source_block           hong18cult
_cod_depositor_comments
'Adding full bibliography for 7700874--7700876.cif.'
_cod_database_code               7700875
_shelx_shelxl_version_number     2014/7
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C35A) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.003
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.003
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.003
Uanis(C16A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.003
3. Others
 Fixed Sof: H15A(0.75) H15B(0.75) H15C(0.25) H15D(0.25) C16(0.75) H16A(0.75)
 H16B(0.75) H16C(0.75) C16A(0.25) H16D(0.25) H16E(0.25) H16F(0.25) C35(0.5)
 H35A(0.5) H35B(0.5) C35A(0.5) H35C(0.5) H35D(0.5) C36(0.5) H36A(0.5) H36B(0.5)
 H36C(0.5) C36A(0.5) H36D(0.5) H36E(0.5) H36F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C15(H15C,H15D), C17(H17A,
 H17B), C19(H19A,H19B), C21(H21A,H21B), C31(H31A,H31B), C33(H33A,H33B),
 C35(H35A,H35B), C35A(H35C,H35D), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C53(H53), C54(H54), C55(H55), C56(H56), C63(H63), C64(H64), C65(H65),
  C66(H66)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C16A(H16D,H16E,
 H16F), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              75975
_olex2_date_sample_data_collection 2018-04-19
_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 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.734