Nonbenzenoid aromaticity of 1-phosphafulvenes: synthesis of phosphacymantrenes.
Liu, Yanjie; Tian, Rongqiang; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 50 (2021) 476–479; doi:10.1039/d0dt03934a

data_7706036
_publ_section_title
;
 Nonbenzenoid aromaticity of 1-phosphafulvenes: synthesis of
 phosphacymantrenes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              476
_journal_page_last               479
_journal_paper_doi               10.1039/d0dt03934a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C59 H48 Mn2 N3 O5 P3'
_chemical_formula_sum            'C59 H48 Mn2 N3 O5 P3'
_chemical_formula_weight         1081.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-20 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                102.356(3)
_cell_angle_beta                 97.645(3)
_cell_angle_gamma                113.816(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0038(6)
_cell_length_b                   13.6029(7)
_cell_length_c                   18.5921(10)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.26
_cell_volume                     2629.9(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47201
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.8350
_exptl_absorpt_correction_T_min  0.7457
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0124(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         12195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0797P)^2^+2.6233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                7295
_reflns_number_total             12195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03934a2.cif
_cod_data_source_block           mo_170721e_0m_sq_d
_cod_depositor_comments
'Adding full bibliography for 7706035--7706039.cif.'
_cod_original_cell_volume        2629.9(2)
_cod_database_code               7706036
_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 Ternary CH refined with riding coordinates:
 C21(H21), C38(H38), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C37(H37), C17(H17), C49(H49), C43(H43), C53(H53), C51(H51),
 C41(H41), C36(H36), C42(H42), C10(H10), C27(H27), C9(H9), C33(H33), C34(H34),
 C26(H26), C35(H35), C6(H6), C25(H25), C8(H8), C18(H18), C7(H7), C50(H50),
 C52(H52), C40(H40), C19(H19), C24(H24)
2.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C59(H59A,H59B,
 H59C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'