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_7704219
_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 Nd2 P4'
_chemical_formula_sum            'C48 H88 B2 Nd2 P4'
_chemical_formula_weight         1099.16
_chemical_name_systematic        '[Nd(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     direct
_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                 93.734(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3618(13)
_cell_length_b                   12.8239(19)
_cell_length_c                   20.685(3)
_cell_measurement_reflns_used    1390
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.9780
_cell_measurement_theta_min      3.3570
_cell_volume                     5389.8(12)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -40.00  50.00   1.00   30.00    --  -18.77  57.00 120.00   90
  2  \w    -51.00  52.00   1.00   30.00    --   20.02 -77.00-120.00  103
;
_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      -0.0109512000
_diffrn_orient_matrix_UB_12      -0.0467736000
_diffrn_orient_matrix_UB_13      0.0140265000
_diffrn_orient_matrix_UB_21      0.0148899000
_diffrn_orient_matrix_UB_22      -0.0293901000
_diffrn_orient_matrix_UB_23      -0.0242325000
_diffrn_orient_matrix_UB_31      0.0295829000
_diffrn_orient_matrix_UB_32      -0.0024743000
_diffrn_orient_matrix_UB_33      0.0199813000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1827
_diffrn_reflns_av_unetI/netI     0.3509
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8100
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.694
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.526
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_preparation       adpm586
_exptl_crystal_recrystallization_method adpm586
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.103
_refine_diff_density_max         3.535
_refine_diff_density_min         -1.693
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     897
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.2540
_refine_ls_R_factor_gt           0.1188
_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^)+(0.1514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2827
_refine_ls_wR_factor_ref         0.3781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1746
_reflns_number_total             4714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01241f2.cif
_cod_data_source_block           1-Nd
_cod_depositor_comments
'Adding full bibliography for 7704215--7704221.cif.'
_cod_original_cell_volume        5389.7(12)
_cod_database_code               7704219
_manchester_internal_diff_code   adpm586
_manchester_internal_coll_client JJL/DPM
_manchester_internal_coll_user   JJL
_manchester_internal_coll_date   29/4/19
_manchester_internal_process_date 29/4/19
_manchester_internal_process_user JJL
_manchester_internal_solution_date 29/4/19
_manchester_internal_solution_user JJL
_manchester_internal_refinement_date 16/7/19
_manchester_internal_refinement_user JJL
_manchester_internal_validation_date 6/11/19
_manchester_internal_validation_user PJC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48B2P4Nd2
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.605
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 B1-H1A = B1-H1B = B1-H1C = B1-H1D
 1.15 with sigma of 0.02
 C14-C13 = C15-C14 = C16-C15 = C4-C3 = C3-C2 = C2-C1
 1.39 with sigma of 0.01
 H1C-H1B \\sim H1D-H1B \\sim H1D-H1C \\sim H1A-H1D \\sim H1A-H1B \\sim H1A-H1C
 with sigma of 0.02
 C4-C2 \\sim C3-C1 \\sim C16-C14 \\sim C15-C13
 with sigma of 0.02
 C24-C23 \\sim C24-C22 \\sim C23-C22 \\sim C24A-C22A \\sim C24A-C23A \\sim
C23A-C22A \\sim C20-C19 ~
 C20A-C19A \\sim C19-C18 \\sim C19A-C18A \\sim C20-C18 \\sim C20A-C18A \\sim
C11-C10 \\sim C12-C10 ~
 C12-C11 \\sim C8-C6 \\sim C8-C7 \\sim C7-C6
 with sigma of 0.02
 C24-C21 \\sim C24A-C21 \\sim C22-C21 \\sim C22A-C21 \\sim C23-C21 \\sim
C23A-C21 \\sim C16-C15 \\sim C20A-
 C17 \\sim C20-C17 \\sim C18A-C17 \\sim C18-C17 \\sim C19A-C17 \\sim C19-C17
\\sim C9-C12 \\sim C9-C11 \\sim C9-
 C10 \\sim C8-C5 \\sim C7-C5 \\sim C6-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
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(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(H23C)=Sof(H23B)=Sof(H23A)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Me refined with riding coordinates:
 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(H23C,H23B,H23A), C24(H24A,
 H24B,H24C), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F),
 C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15)
;
_shelx_res_checksum              59894
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.203
_oxdiff_exptl_absorpt_empirical_full_min 0.236