Homoleptic uranium and lanthanide phosphinodiboranates.
Blake, Anastasia V.; Fetrow, Taylor V.; Theiler, Zachary J.; Vlaisavljevich, Bess; Daly, Scott R.; Chemical communications (Cambridge, England) 54 (2018) 5602–5605; doi:10.1039/c8cc02862a

data_7121685
_publ_section_title
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 Homoleptic uranium and lanthanide phosphinodiboranates.
;
_journal_issue                   44
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5602
_journal_page_last               5605
_journal_paper_doi               10.1039/c8cc02862a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C48 H144 B12 Nd2 P6, C4 H10 O'
_chemical_formula_sum            'C52 H154 B12 Nd2 O P6'
_chemical_formula_weight         1399.76
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-04-28 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.050(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0204(15)
_cell_length_b                   11.9884(12)
_cell_length_c                   24.771(2)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.1735
_cell_volume                     4460.5(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67308
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         2.324
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0792 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.8744.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         9136
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0917P)^2^+13.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6491
_reflns_number_total             9136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02862a8.cif
_cod_data_source_block           dal1744
_cod_depositor_comments
'Adding full bibliography for 7121683--7121685.cif.'
_cod_database_code               7121685
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C71-C72 = C74-C75
 1.54 with sigma of 0.01
 O73-C72 = O73-C74
 1.43 with sigma of 0.01
 H42C-H33A
 1.85 with sigma of 0.01
 C11-C12 \\sim C11-C13 \\sim C11-C14 \\sim C21-C22 \\sim C21-C23 \\sim C21-C24
\\sim C31-C32 \\sim C31-C33
 \\sim C31-C34
 with sigma of 0.01
 C41-C42 \\sim C41-C43 \\sim C41-C44 \\sim C51-C52 \\sim C51-C53 \\sim C51-C54
\\sim C61-C62 \\sim C61-C63
 \\sim C61-C64
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14)
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34)
Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44)
Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54)
Uanis(C71) = Uanis(C72) = Uanis(O73) = Uanis(C74) = Uanis(C75)
4. Others
 Fixed Sof: C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) O73(0.5) C74(0.5) H74A(0.5)
 H74B(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C72(H72A,H72B)
5.b Me refined with riding coordinates:
 C75(H75A,H75B,H75C), C71(H71A,H71B,H71C)
5.c Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B5(H5A,
 H5B,H5C), B6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,
 H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C)
;
_shelx_res_checksum              76087
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'