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_7704215
_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         'C48 H88 B2 Ce2 P4'
_chemical_formula_sum            'C48 H88 B2 Ce2 P4'
_chemical_formula_weight         1090.92
_chemical_name_systematic        '[Ce(Htp)2(BH4)]2'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-06
_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                 91.935(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.647(3)
_cell_length_b                   12.9366(9)
_cell_length_c                   20.2887(17)
_cell_measurement_reflns_used    1218
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.0830
_cell_measurement_theta_min      4.0010
_cell_volume                     5416.1(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -91.00 -11.00   1.00    1.50    --  -44.20 -57.00  30.00   80
  2  \w    -78.00   8.00   1.00    1.50    --  -44.20  57.00-120.00   86
  3  \w   -128.00  28.00   1.00    1.50    --  -44.20 -19.00  60.00  156
  4  \w   -133.00-104.00   1.00    1.50    --  -44.20 -57.00  30.00   29
  5  \w    -80.00  45.00   1.00    1.50    --  -44.20  76.00 -60.00  125
  6  \w    -71.00 -28.00   1.00    7.00    -- -110.00  76.00  30.00   43
  7  \w   -150.00 -37.00   1.00    7.00    -- -110.00  76.00-150.00  113
  8  \w   -193.00 -37.00   1.00    7.00    -- -110.00   0.00-180.00  156
  9  \w   -143.00 -49.00   1.00    7.00    -- -110.00  76.00 -90.00   94
 10  \w   -197.00 -80.00   1.00    7.00    -- -110.00 -57.00 -30.00  117
 11  \w   -188.00 -31.00   1.00    7.00    -- -110.00  19.00 -30.00  157
 12  \w   -149.00 -75.00   1.00    7.00    -- -110.00  76.00  30.00   74
 13  \w   -148.00 -21.00   1.00    7.00    -- -110.00  76.00 120.00  127
 14  \w   -150.00 -24.00   1.00    7.00    -- -110.00  76.00  60.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0042474000
_diffrn_orient_matrix_UB_12      0.0438503000
_diffrn_orient_matrix_UB_13      0.0703902000
_diffrn_orient_matrix_UB_21      0.0262139000
_diffrn_orient_matrix_UB_22      0.1044990000
_diffrn_orient_matrix_UB_23      -0.0238042000
_diffrn_orient_matrix_UB_31      -0.0697111000
_diffrn_orient_matrix_UB_32      0.0368188000
_diffrn_orient_matrix_UB_33      -0.0158877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1205
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23912
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.134
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.244
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.095
_refine_diff_density_max         2.460
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0925
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+8.8064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2215
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3538
_reflns_number_total             4950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           1-Ce
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_original_cell_volume        5416.1(9)
_cod_database_code               7704215
_manchester_internal_diff_code   rdpm163
_manchester_internal_coll_client FO/JJL
_manchester_internal_coll_user   FO/JJL
_manchester_internal_coll_date   1/10/18
_manchester_internal_process_date 1/10/18
_manchester_internal_process_user FO/JJL
_manchester_internal_solution_date 1/10/18
_manchester_internal_solution_user FO/JJL
_manchester_internal_refinement_date 28/11/18
_manchester_internal_refinement_user JJL
_manchester_internal_validation_date 5/11/19
_manchester_internal_validation_user PJC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ce2B4P4C48
_shelx_estimated_absorpt_t_max   0.347
_shelx_estimated_absorpt_t_min   0.209
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.974(2)
 0.026(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H,H) groups, All C(H,H,H) groups
3. Restrained distances
 B1-H1D = B1-H1B = B1-H1A = B1-H1C
 1.15 with sigma of 0.01
 H1D-H1B = H1D-H1C = H1A-H1B = H1A-H1D = H1C-H1B = H1C-H1A
 1.95 with sigma of 0.01
 C2-C1 \\sim C3-C2 \\sim C4-C3 \\sim C14-C13 \\sim C15-C14 \\sim C16-C15
 with sigma of 0.01
 C15-C13 \\sim C16-C14 \\sim C4-C2 \\sim C3-C1
 with sigma of 0.02
4. Restrained planarity
 P1, C1, C2, C3, C4
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15)
6.b Idealised Me refined as rotating group:
 C00M(H00A,H00B,H00C), 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), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              47876
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 0.5s
_manchester_internal_coll_frame_width 0.5
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.128
_oxdiff_exptl_absorpt_empirical_full_min 0.517