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_7704217
_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 La2 P4'
_chemical_formula_sum            'C48 H88 B2 La2 P4'
_chemical_formula_weight         1088.588
_chemical_name_systematic        '[La(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'
_symmetry_Int_Tables_number      15
_audit_creation_date             2020-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-24 deposited with the CCDC.	2020-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.015(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7897(10)
_cell_length_b                   12.9165(4)
_cell_length_c                   20.3007(6)
_cell_measurement_reflns_used    2023
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      58.6420
_cell_measurement_theta_min      4.0110
_cell_volume                     5448.0(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      159(2)
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_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    -33.00  26.00   0.50    1.50    --  -44.30  39.00  99.00  118
  2  \w   -133.00  -7.00   0.50    1.50    --  -44.30 -39.00 -55.00  252
  3  \w   -164.00-113.00   0.50    1.50    -- -110.00 -39.00 -55.00  102
  4  \w   -105.00 -30.00   0.50    1.50    -- -110.00  39.00  99.00  150
  5  \w    -78.00  16.00   0.50    1.50    --  -44.30  57.00-120.00  188
  6  \w   -148.00 -23.00   0.50    1.50    -- -110.00  76.00  90.00  250
  7  \w   -143.00 -56.00   0.50    1.50    -- -110.00  57.00 -90.00  174
  8  \w    -52.00 -22.00   0.50    1.50    -- -110.00  57.00 -90.00   60
  9  \w   -163.00-132.00   0.50    1.50    -- -110.00  19.00 -60.00   62
 10  \w   -131.00 -27.00   0.50    1.50    -- -110.00  19.00 -60.00  208
 11  \w   -150.00 -22.00   0.50    1.50    -- -110.00  38.00 -60.00  256
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9977
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15175
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9977
_diffrn_reflns_theta_full        66.5998
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    13.257
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.259
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             2244.616
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.087
_refine_diff_density_max         4.0132
_refine_diff_density_min         -1.4382
_refine_diff_density_rms         0.2307
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             10.9695
_refine_ls_goodness_of_fit_ref   1.0628
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    73
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.0490
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1519P)^2^+62.9369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2657
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                4005
_reflns_number_total             4809
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           1-La
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc (x+z,y,-x)'
_cod_database_code               7704217
_manchester_internal_diff_code   rdpm168
_manchester_internal_coll_client FO/JJL
_manchester_internal_coll_user   FO/JJL
_manchester_internal_coll_date   10/5/19
_manchester_internal_process_date 10/5/19
_manchester_internal_process_user JJL
_manchester_internal_solution_date 10/5/19
_manchester_internal_solution_user JJL
_manchester_internal_refinement_date 23/3/20
_manchester_internal_refinement_user FO/PJC
_manchester_internal_validation_date 23/3/20
_manchester_internal_validation_user PJC/FO
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C3-C2 = C4-C3 = C2-C1
 1.39 with sigma of 0.01
 B1-H1c = B1-H1d = B1-H1a = B1-H1b
 1.15 with sigma of 0.02
 C15-C13 \\sim C16-C14 \\sim C4-C2 \\sim C3-C1
 with sigma of 0.02
 C6-C5 \\sim C8A-C5 \\sim C8-C5 \\sim C7A-C5 \\sim C7-C5 \\sim C6A-C5 \\sim
C20-C17 \\sim C18-C17 \\sim C19-
 C17 \\sim C9-C11 \\sim C9-C10 \\sim C9-C12 \\sim C24-C21 \\sim C23-C21 \\sim
C22-C21
 with sigma of 0.02
 C8A-C7A \\sim C7A-C6A \\sim C8A-C6A \\sim C12-C10 \\sim C8-C6 \\sim C8-C7
\\sim C7-C6 \\sim C12-C11 \\sim C11-
 C10 \\sim C20-C19 \\sim C20-C18 \\sim C19-C18 \\sim C24-C22 \\sim C24-C23
\\sim C23-C22
 with sigma of 0.02
 H1a-H1b \\sim H1a-H1c \\sim H1a-H1d \\sim H1b-H1c \\sim H1b-H1d \\sim H1c-H1d
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim P1 \\sim C1 \\sim C5 \\sim C8A \\sim C8 \\sim C7A
\\sim C7 \\sim C6 \\sim C6A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=Sof(H7Ac)=Sof(C6A)=Sof(H6Aa)=Sof(H6Ab)=Sof(H6Ac)=
 Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(H8Ac)=1-FVAR(1)
 Sof(C7)=Sof(H7a)=Sof(H7b)=Sof(H7c)=Sof(C8)=Sof(H8a)=Sof(H8b)=Sof(H8c)=Sof(C6)=
 Sof(H6a)=Sof(H6b)=Sof(H6c)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C14(H14), C2(H2), C3(H3)
6.b Me refined with riding coordinates:
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C18(H18a,H18b,
 H18c), C20(H20a,H20b,H20c), C12(H12a,H12b,H12c), C11(H11a,H11b,H11c), C19(H19a,
 H19b,H19c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C6(H6a,H6b,H6c), C10(H10a,H10b,
 H10c), C7A(H7Aa,H7Ab,H7Ac), C6A(H6Aa,H6Ab,H6Ac), C8A(H8Aa,H8Ab,H8Ac)
;
_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
;