F-element metalated dipyrrins: synthesis and characterization of a family of uranyl bis(dipyrrinate) complexes.
Bolotaulo, Duer; Metta-Magaña, Alejandro; Fortier, Skye; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3284–3294; doi:10.1039/c7dt00150a

data_7042055
_publ_section_title
;
 F-element metalated dipyrrins: synthesis and characterization of a family
 of uranyl bis(dipyrrinate) complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3284
_journal_page_last               3294
_journal_paper_doi               10.1039/c7dt00150a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '2(C36 H34 N4 O5 U), C4 O, 1.4(C5)'
_chemical_formula_sum            'C90 H78 N8 O11 U2'
_chemical_formula_weight         1923.66
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-01-09 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                99.0510(10)
_cell_angle_beta                 103.8570(10)
_cell_angle_gamma                98.0330(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5004(7)
_cell_length_b                   16.3863(8)
_cell_length_c                   16.7499(9)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.429
_cell_measurement_theta_min      2.258
_cell_volume                     3750.1(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41352
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         1.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.384
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0906 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.7725.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'red orange'
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.230
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         17045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12380
_reflns_number_total             17045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00150a2.cif
_cod_data_source_block           1113SF
_cod_depositor_comments
'Adding full bibliography for 7042053--7042056.cif.'
_cod_database_code               7042055
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C70(H70A,H70B), C69(H69A,H69B), C34(H34A,H34B), C33(H33A,
 H33B), C36(H36A,H36B), C71(H71A,H71B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C18(H18), C2(H2), C1(H1), C23(H23), C58(H58), C48(H48), C50(H50),
 C59(H59), C54(H54), C67(H67), C22(H22), C53(H53), C64(H64), C27(H27), C16(H16),
  C51(H51), C37(H37), C3(H3), C39(H39), C38(H38), C17(H17), C57(H57), C32(H32),
 C11(H11), C55(H55), C63(H63), C43(H43), C65(H65), C7(H7), C28(H28), C31(H31),
 C30(H30), C14(H14), C10(H10), C13(H13), C47(H47), C44(H44), C15(H15), C8(H8)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C68(H68A,H68B,H68C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              74064
_olex2_submission_special_instructions 'No special instructions were received'