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_7704216
_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 P4 Sm2'
_chemical_formula_sum            'C48 H88 B2 P4 Sm2'
_chemical_formula_weight         1111.38
_chemical_name_systematic        '[Sm(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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-07
_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                 94.177(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4242(11)
_cell_length_b                   12.8734(9)
_cell_length_c                   20.6935(18)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      57.0130
_cell_measurement_theta_min      3.9760
_cell_volume                     5426.5(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     17.00  42.00   1.00    5.00    --   44.80  30.00   0.00   25
  2  \w    -40.00 -13.00   1.00    5.00    --   44.80  30.00   0.00   27
  3  \w    -45.00 131.00   1.00    5.00    --   44.80  10.00  90.00  176
  4  \w     83.00 128.00   1.00    5.00    --   44.80  30.00   0.00   45
  5  \w     91.00 155.00   1.00   10.00    --  108.00  50.00 -90.00   64
  6  \w     71.00 196.00   1.00   10.00    --  108.00  50.00   0.00  125
  7  \w     46.00  81.00   1.00   10.00    --  108.00  50.00 -90.00   35
  8  \w    129.00 193.00   1.00   10.00    --  108.00  10.00 120.00   64
  9  \w     77.00 103.00   1.00   10.00    --  108.00   0.00-180.00   26
 10  \w    124.00 152.00   1.00   10.00    --  108.00   0.00-180.00   28
 11  \w     19.00  71.00   1.00   10.00    --  108.00  40.00   0.00   52
 12  \w     88.00 191.00   1.00   10.00    --  108.00  40.00   0.00  103
 13  \w     19.00 113.00   1.00   10.00    --  108.00  10.00 120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0728276000
_diffrn_orient_matrix_UB_12      0.0138848000
_diffrn_orient_matrix_UB_13      0.0234265000
_diffrn_orient_matrix_UB_21      -0.0204507000
_diffrn_orient_matrix_UB_22      0.0446106000
_diffrn_orient_matrix_UB_23      0.0646255000
_diffrn_orient_matrix_UB_31      0.0008742000
_diffrn_orient_matrix_UB_32      -0.1101314000
_diffrn_orient_matrix_UB_33      0.0291019000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         4.047
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    17.394
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.558
_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    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.824
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     799
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1357P)^2^+9.3267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2640
_reflns_number_total             4784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           1-Sm
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_database_code               7704216
_manchester_internal_diff_code   ldpm85
_manchester_internal_coll_client JJL
_manchester_internal_coll_user   JJL
_manchester_internal_coll_date   5/12/18
_manchester_internal_process_date 5/12/18
_manchester_internal_process_user JJL
_manchester_internal_solution_date 5/12/18
_manchester_internal_solution_user JJL
_manchester_internal_refinement_date 5/12/18
_manchester_internal_refinement_user JJL
_manchester_internal_validation_date 7/11/19
_manchester_internal_validation_user PJC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24BSmP2
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C15-C14 = C16-C15 = C14-C13 = C2-C1 = C3-C2 = C4-C3
 1.39 with sigma of 0.01
 B1-H1A = B1-H1B = B1-H1D = B1-H1C
 1.15 with sigma of 0.02
 C17-C13 \\sim C21-C16 \\sim C5-C1 \\sim C9-C4
 with sigma of 0.02
 C20A-C17 \\sim C18A-C17 \\sim C18-C17 \\sim C20-C17 \\sim C19A-C17 \\sim
C19-C17 \\sim C23-C21 \\sim C24-
 C21 \\sim C22-C21 \\sim C9-C12 \\sim C9-C10 \\sim C9-C11 \\sim C8-C5 \\sim
C7-C5 \\sim C6-C5 \\sim C23A-C21 ~
 C22A-C21 \\sim C24A-C21
 with sigma of 0.02
 C8-C7 \\sim C7-C6 \\sim C8-C6 \\sim C12-C11 \\sim C11-C10 \\sim C12-C10 \\sim
C20A-C19A \\sim C20A-C18A ~
 C19A-C18A \\sim C20-C18 \\sim C20-C19 \\sim C19-C18 \\sim C23-C22 \\sim
C24-C22 \\sim C24-C23 \\sim C24A-
 C23A \\sim C24A-C22A \\sim C23A-C22A
 with sigma of 0.02
 H1D-H1A \\sim H1C-H1A \\sim H1A-H1B \\sim H1D-H1B \\sim H1C-H1B \\sim H1C-H1D
 with sigma of 0.02
 C4-C2 \\sim C3-C1 \\sim C15-C13 \\sim C16-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C23 \\sim C22A \\sim C21 \\sim C24A \\sim C24 \\sim C23A \\sim C22 \\sim C16
\\sim C15 \\sim C14 \\sim P2 \\sim C13 \\sim C19 \\sim C20A \\sim C19A \\sim
C17 \\sim C18 \\sim C18A \\sim C20 \\sim C8 \\sim C5 \\sim C6 \\sim C7 \\sim
C12 \\sim C9 \\sim C10 \\sim C11 \\sim C4 \\sim C2 \\sim C3 \\sim C1 \\sim P1:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 P2, C23, C22A, C21, C24A, C24, C23A, C22, C16, C15, C14, P2, C13, C19, C20A,
 C19A, C17, C18, C18A, C20, C8, C5, C6, C7, C12, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15)
6.b Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C22A(H22D,H22E,
 H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
6.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), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F),
 C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              70369
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_frame_time 3s
_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 2.315
_oxdiff_exptl_absorpt_empirical_full_min 0.477