Cerium-carbon dative interactions supported by carbodiphosphorane.
Su, Wei; Pan, Sudip; Sun, Xiong; Zhao, Lili; Frenking, Gernot; Zhu, Congqing; Dalton transactions (Cambridge, England : 2003) 48 (2019) 16108–16114; doi:10.1039/c9dt03770e

data_7701302
_publ_section_title
;
 Cerium-carbon dative interactions supported by carbodiphosphorane.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16108
_journal_page_last               16114
_journal_paper_doi               10.1039/c9dt03770e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C70 H56 Br Ce N4 P4, 2(C24 H20 B)'
_chemical_formula_sum            'C118 H96 B2 Br Ce N4 P4'
_chemical_formula_weight         1935.51
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-06-10 deposited with the CCDC.    2019-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.62
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.131
_cell_length_b                   30.502
_cell_length_c                   19.646
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    193.01
_cell_measurement_theta_max      54.010
_cell_measurement_theta_min      2.319
_cell_volume                     9933.230
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1390
_diffrn_reflns_av_unetI/netI     0.1205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            86025
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.010
_diffrn_reflns_theta_min         2.319
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.307
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1438 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.6837.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             3980
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         18140
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0783P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9448
_reflns_number_total             18140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03770e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7701300--7701303.cif.'
_cod_original_cell_volume        9932.7
_cod_database_code               7701302
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.558
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(H21a)=Sof(N4)=Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=
 1-FVAR(1)
 Sof(N4A)=Sof(H21)=Sof(C24)=Sof(H24)=Sof(C23)=Sof(H23)=Sof(C22)=Sof(H22)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C81(H81), C80(H80), C108(H108), C82(H82), C26(H26), C61(H61),
 C40(H40), C96(H96), C9(H9), C109(H109), C104(H104), C3(H3), C33(H33), C16(H16),
  C34(H34), C70(H70), C66(H66), C114(H114), C91(H91), C99(H99), C47(H47),
 C63(H63), C94(H94), C93(H93), C90(H90), C32(H32), C110(H110), C49(H49), C6(H6),
  C52(H52), C36(H36), C106(H106), C29(H29), C45(H45), C35(H35), C64(H64),
 C30(H30), C76(H76), C39(H39), C73(H73), C102(H102), C100(H100), C15(H15),
 C38(H38), C10(H10), C118(H118), C116(H116), C103(H103), C68(H68), C105(H105),
 C43(H43), C11(H11), C46(H46), C67(H67), C55(H55), C112(H112), C57(H57),
 C12(H12), C53(H53), C56(H56), C13(H13), C44(H44), C78(H78), C60(H60), C37(H37),
  C84(H84), C62(H62), C72(H72), C74(H74), C21(H21), C21(H21a), C117(H117),
 C115(H115), C69(H69), C51(H51), C111(H111), C98(H98), C5(H5), C79(H79),
 C88(H88), C28(H28), C75(H75), C27(H27), C87(H87), C86(H86), C97(H97), C17(H17),
  C85(H85), C50(H50), C54(H54), C92(H92), C24(H24), C23(H23), C22(H22),
 C19(H19), C18(H18), C24A(H24A), C23A(H23A), C22A(H22A)
;
_olex2_submission_special_instructions 'No special instructions were received'