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_7704218
_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 K2 La2 O8 P4'
_chemical_formula_sum            'C64 H136 B4 K2 La2 O8 P4'
_chemical_formula_weight         1556.86
_chemical_name_systematic        '[La(Htp)2(BH4)2K(DME)2]2'
_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                 98.041(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6790(2)
_cell_length_b                   21.0788(4)
_cell_length_c                   18.7550(5)
_cell_measurement_reflns_used    14004
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1290
_cell_measurement_theta_min      2.0600
_cell_volume                     4180.25(16)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  88.00   0.50    0.50    --   -0.50  62.00 111.00  242
  2  \w     10.00  35.00   0.50    1.00    --    5.00  62.00 110.00   50
  3  \w     45.00  74.00   0.50    1.00    --   -8.30  57.00-180.00   58
  4  \w    -42.00  81.00   0.50    1.00    --   -8.30  57.00  30.00  246
  5  \w    -35.00  21.00   0.50    1.00    --   -8.30  57.00-180.00  112
;
_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      0.0192732000
_diffrn_orient_matrix_UB_12      0.0181344000
_diffrn_orient_matrix_UB_13      0.0314704000
_diffrn_orient_matrix_UB_21      -0.0585916000
_diffrn_orient_matrix_UB_22      0.0163605000
_diffrn_orient_matrix_UB_23      -0.0052407000
_diffrn_orient_matrix_UB_31      -0.0264368000
_diffrn_orient_matrix_UB_32      -0.0231405000
_diffrn_orient_matrix_UB_33      0.0209830000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40661
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         1.461
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.553
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7657
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.9841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6269
_reflns_number_total             7657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           2-La
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_original_cell_volume        4180.24(17)
_cod_database_code               7704218
_manchester_internal_diff_code   rdpm153
_manchester_internal_coll_client FO/JJL
_manchester_internal_coll_user   FO/JJL
_manchester_internal_coll_date   19/9/18
_manchester_internal_process_date 19/9/18
_manchester_internal_process_user FO/JJL
_manchester_internal_solution_date 19/9/18
_manchester_internal_solution_user FO/JJL
_manchester_internal_refinement_date 19/9/18
_manchester_internal_refinement_user JJL
_manchester_internal_validation_date 08/11/19
_manchester_internal_validation_user PJC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         LaC32H68B2KO4P2
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.731
_reflns_odcompleteness_completeness 99.90
_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 B(H,H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 B1-H1B = B1-H1C = B1-H1D = B1-H1A = B2-H2C = B2-H2D = B2-H2B = B2-H2A
 1.15 with sigma of 0.02
3. 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)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C26A(H26C,H26D), C27(H27A,H27B), C27A(H27C,H27D), C30(H30A,
 H30B), C31(H31A,H31B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15)
4.c 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), C29(H29A,H29B,H29C),
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              16661
_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 4.324
_oxdiff_exptl_absorpt_empirical_full_min 0.508