Synthesis and characterisation of light lanthanide bis-phospholyl borohydride complexes.
Liu, Jingjing; Nodaraki, Lydia E.; Cobb, Philip J.; Giansiracusa, Marcus J.; Ortu, Fabrizio; Tuna, Floriana; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6504–6511; doi:10.1039/d0dt01241f

data_7704220
_publ_section_title
;
 Synthesis and characterisation of light lanthanide bis-phospholyl
 borohydride complexes.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6504
_journal_page_last               6511
_journal_paper_doi               10.1039/d0dt01241f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C64 H136 B4 Ce2 K2 O8 P4'
_chemical_formula_sum            'C64 H136 B4 Ce2 K2 O8 P4'
_chemical_formula_weight         1559.28
_chemical_name_systematic        '[Ce(Htp)2(BH4)2K(DME)2]2'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.442(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6463(4)
_cell_length_b                   21.0099(9)
_cell_length_c                   18.7079(8)
_cell_measurement_reflns_used    5279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.8350
_cell_measurement_theta_min      2.9230
_cell_volume                     4139.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -95.00 -60.00   1.00   15.00    --  -18.77-178.00 -60.00   35
  2  \w    -20.00  24.00   1.00   15.00    --  -18.77 -99.00-150.00   44
  3  \w     12.00  42.00   1.00   15.00    --   20.02 -57.00  60.00   30
  4  \w    -42.00  -9.00   1.00   15.00    --   20.02 -57.00  60.00   33
  5  \w     39.00  80.00   1.00   15.00    --   20.02 178.00  30.00   41
  6  \w    -39.00  66.00   1.00   15.00    --   20.02 -19.00-120.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0059537000
_diffrn_orient_matrix_UB_12      -0.0302664000
_diffrn_orient_matrix_UB_13      -0.0159883000
_diffrn_orient_matrix_UB_21      -0.0039807000
_diffrn_orient_matrix_UB_22      0.0145430000
_diffrn_orient_matrix_UB_23      -0.0344781000
_diffrn_orient_matrix_UB_31      0.0669431000
_diffrn_orient_matrix_UB_32      0.0035704000
_diffrn_orient_matrix_UB_33      0.0049958000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.739
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       needle
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.504
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7572
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5693
_reflns_number_total             7572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           2-Ce
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_database_code               7704220
_manchester_internal_diff_code   adpm514
_manchester_internal_coll_client JJL
_manchester_internal_coll_user   JJL
_manchester_internal_coll_date   13/9/18
_manchester_internal_process_date 13/9/18
_manchester_internal_process_user JJL
_manchester_internal_solution_date 13/9/18
_manchester_internal_solution_user JJL
_manchester_internal_refinement_date 13/9/18
_manchester_internal_refinement_user JJL
_manchester_internal_validation_date 8/11/19
_manchester_internal_validation_user PJC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CeKC28P2B2O2
_chemical_oxdiff_usercomment     'RP535 pentane layer'
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.559
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 B2-H2C = B2-H2B = B2-H2A = B2-H2D = B1-H1C = B1-H1D = B1-H1A = B1-H1B
 1.15 with sigma of 0.02
 O1-C26 \\sim O1-C26A \\sim O2-C27A \\sim O2-C27 \\sim O4-C31 \\sim O3-C30
 with sigma of 0.02
 C31-C30 \\sim C27A-C26A \\sim C27-C26
 with sigma of 0.02
 O2-C28 \\sim O1-C25 \\sim O4-C32 \\sim O3-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28 \\sim O2 \\sim C27A \\sim C26 \\sim C27 \\sim C26A \\sim O1 \\sim C25:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C28, O2, C27, C27A, C26A, C26, C25, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C26(H26A,H26B), C27(H27A,H27B), C26A(H26C,
 H26D), C27A(H27C,H27D)
6.c Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C32(H32A,H32B,H32C)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              72746
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 3.5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_type   custom
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.660