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_7042053
_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
'C36 H34 N4 O3 U, C36 H28 N4 O3 U, C4 O, C3 O0.5, C1.83 O0.33'
_chemical_formula_sum            'C80 H84 N4 O8 U2'
_chemical_formula_weight         1705.57
_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     heavy
_atom_sites_solution_secondary   difmap
_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                98.7660(10)
_cell_angle_beta                 102.5540(10)
_cell_angle_gamma                96.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4946(5)
_cell_length_b                   15.8228(5)
_cell_length_c                   16.5676(5)
_cell_measurement_reflns_used    7797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.181
_cell_measurement_theta_min      2.160
_cell_volume                     3618.4(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.986
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39775
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.7735.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'red orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.364
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         16322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+5.0086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                11584
_reflns_number_total             16322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00150a2.cif
_cod_data_source_block           1098SF
_cod_depositor_comments
'Adding full bibliography for 7042053--7042056.cif.'
_cod_database_code               7042053
_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. Others
 Fixed Sof: C35A(0.5) O8(0.5) C35B(0.5) O9(0.33333) C83(0.33333) C82(0.33333)
 C81(0.33333) C80(0.33333) C100(0.25) C101(0.25)
3.a Free rotating group:
 O9(C83,C82,C81,C80)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C71(H71A,H71B), C72(H72A,H72B), C69(H69A,H69B), C70(H70A,H70B),
 C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C43(H43), C45(H45), C66(H66), C59(H59), C44(H44), C11(H11), C7(H7),
 C39(H39), C48(H48), C47(H47), C25(H25), C9(H9), C38(H38), C50(H50), C19(H19),
 C51(H51), C55(H55), C31(H31), C37(H37), C12(H12), C53(H53), C64(H64), C54(H54),
  C1(H1), C60(H60), C18(H18), C8(H8), C23(H23), C30(H30), C17(H17), C61(H61),
 C15(H15), C24(H24), C67(H67), C14(H14), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C68(H68A,H68B,H68C), C16(H16A,H16B,H16C), C32(H32A,H32B,
 H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'