Probing a variation of the inverse-trans-influence in americium and lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes
Windorff, Cory J.; Celis-Barros, Cristian; Sperling, Joseph M.; McKinnon, Noah C.; Albrecht-Schmitt, Thomas E.; Chemical Science 11 (2020) 2770–2782; doi:10.1039/C9SC05268B

data_1557255
_publ_section_title
;
 Probing a variation of the inverse-trans-influence in americium and
 lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              2770
_journal_page_last               2782
_journal_paper_doi               10.1039/C9SC05268B
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C54 H99 Br3 Ce O3 P3'
_chemical_formula_sum            'C54 H99 Br3 Ce O3 P3'
_chemical_formula_weight         1269.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-16 deposited with the CCDC.	2020-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.920(5)
_cell_length_b                   11.434(2)
_cell_length_c                   18.209(3)
_cell_measurement_reflns_used    9514
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.438
_cell_measurement_theta_min      2.531
_cell_volume                     6021.2(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            122286
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.864
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0972 before and 0.0803 after correction. The Ratio of minimum to maximum transmission is 0.8648. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             2620
_exptl_crystal_preparation       'mixture of components in isopropyl alcohol'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: iPrOH'
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 5009 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         13805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0145P)^2^+11.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11775
_reflns_number_total             13805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05268b2.cif
_cod_data_source_block           'save_b_CCDC1'
_cod_depositor_comments
;Adding full bibliography for 1557253--1557257.cif.

 Adding full bibliography for 1557253--1557257.cif.
;
_cod_database_code               1557255
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.514
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.964(10)
 0.036(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C25(H25), C19(H19), C7(H7), C1(H1), C13(H13), C31(H31), C37(H37), C43(H43),
 C49(H49)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C30(H30A,H30B), C44(H44A,H44B), C48(H48A,H48B), C36(H36A,H36B),
 C17(H17A,H17B), C3(H3A,H3B), C27(H27A,H27B), C26(H26A,H26B), C21(H21A,H21B),
 C32(H32A,H32B), C9(H9A,H9B), C8(H8A,H8B), C15(H15A,H15B), C14(H14A,H14B),
 C20(H20A,H20B), C28(H28A,H28B), C12(H12A,H12B), C29(H29A,H29B), C35(H35A,H35B),
  C46(H46A,H46B), C5(H5A,H5B), C22(H22A,H22B), C18(H18A,H18B), C10(H10A,H10B),
 C50(H50A,H50B), C4(H4A,H4B), C6(H6A,H6B), C16(H16A,H16B), C47(H47A,H47B),
 C0AA(H0AA,H0AB), C45(H45A,H45B), C23(H23A,H23B), C41(H41A,H41B), C42(H42A,
 H42B), C24(H24A,H24B), C11(H11A,H11B), C38(H38A,H38B), C52(H52A,H52B),
 C34(H34A,H34B), C39(H39A,H39B), C40(H40A,H40B), C51(H51A,H51B), C53(H53A,H53B),
  C33(H33A,H33B)
;
_shelx_res_checksum              31
_olex2_exptl_crystal_mounting_method 'nylon lopp'
_olex2_submission_original_sample_id cjw63
_olex2_submission_special_instructions 'No special instructions were received'