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_7042054
_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         'C43 H44 N6 O2 U, C4 O, C3'
_chemical_formula_sum            'C56 H73 N6 O3 U'
_chemical_formula_weight         1116.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 102.9630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3522(6)
_cell_length_b                   26.9204(16)
_cell_length_c                   18.8537(11)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.546
_cell_measurement_theta_min      2.217
_cell_volume                     4625.7(5)
_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      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56102
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.478
_diffrn_reflns_theta_min         1.513
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.563
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1220 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.5790.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.650
_refine_diff_density_min         -5.477
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         13066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0083P)^2^+32.4491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10844
_reflns_number_total             13066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00150a2.cif
_cod_data_source_block           1295SF
_cod_depositor_comments
'Adding full bibliography for 7042053--7042056.cif.'
_cod_database_code               7042054
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C40(H40), C37(H37), C17(H17), C18(H18), C39(H39), C31(H31), C1(H1),
 C26(H26), C16(H16), C20(H20), C3(H3), C25(H25), C21(H21), C19(H19), C27(H27),
 C34(H34), C9(H9), C2(H2), C12(H12)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C11(H11A,H11B,
 H11C), C42(H42A,H42B,H42C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C43(H43A,
 H43B,H43C)
;
_shelx_res_checksum              68604
_olex2_submission_special_instructions 'No special instructions were received'