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_7121683
_publ_section_title
;
 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 Er2 P6'
_chemical_formula_sum            'C48 H144 B12 Er2 P6'
_chemical_formula_weight         1371.68
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-04-07 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.557(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7928(15)
_cell_length_b                   12.1704(12)
_cell_length_c                   24.504(2)
_cell_measurement_reflns_used    16051
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.00
_cell_volume                     4409.9(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1561
_diffrn_reflns_av_unetI/netI     0.1283
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31095
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.589
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.289
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         8646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4706
_reflns_number_total             8646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02862a8.cif
_cod_data_source_block           dal1761
_cod_depositor_comments
'Adding full bibliography for 7121683--7121685.cif.'
_cod_database_code               7121683
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34)
Uanis(C62) = Uanis(C63) = Uanis(C64)
3.a Me refined with riding coordinates:
 C14(H14A,H14B,H14C)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), 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), B1(H1A,H1B,H1C), B2(H2A,H2B,
 H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B5(H5A,H5B,H5C), B6(H6A,H6B,H6C)
;
_shelx_res_checksum              28483
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'