Substituent effects in pyridyl-functionalized pyrylium salts, pyridines and λ<sup>3</sup>,σ<sup>2</sup>-phosphinines: a fundamental and systematic study.
Loibl, Antonia; Oschmann, Wiebke; Vogler, Maria; Pidko, Evgeny A.; Weber, Manuela; Wiecko, Jelena; Müller, Christian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9355–9366; doi:10.1039/c8dt01441h

data_7046653
_publ_section_title
;
 Substituent effects in pyridyl-functionalized pyrylium salts, pyridines
 and \l<sup>3</sup>,\s<sup>2</sup>-phosphinines: a fundamental and
 systematic study.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9355
_journal_page_last               9366
_journal_paper_doi               10.1039/c8dt01441h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C27 H15 F3 N2 O4 W)'
_chemical_formula_sum            'C54 H30 F6 N4 O8 W2'
_chemical_formula_weight         1344.52
_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
_audit_creation_date             2014-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3220(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5198(7)
_cell_length_b                   17.2400(9)
_cell_length_c                   19.1014(10)
_cell_measurement_reflns_used    9507
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.552
_cell_measurement_theta_min      2.877
_cell_volume                     4718.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78726
_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         30.563
_diffrn_reflns_theta_min         2.254
_exptl_absorpt_coefficient_mu    4.958
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1383 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.4587.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         14451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+5.4192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13202
_reflns_number_total             14451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01441h2.cif
_cod_data_source_block           al176_a
_cod_depositor_comments
'Adding full bibliography for 7046645--7046658.cif.'
_cod_database_code               7046653
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C29(H29),
  C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49)
;
_shelx_res_checksum              78172
_olex2_submission_special_instructions 'No special instructions were received'