3-(Dialkoxyphosphoryl)-N-confused Phlorin and Porphyrin. Synthesis, Stereochemistry, and Coordination Properties
Bin Liu; Xiaofang Li; Xin Xu; Marcin Stępień; Piotr J. Chmielewski; Journal of Organic Chemistry 78 (2013) 1354–1364; doi:10.1021/jo302689d

data_4027966
_publ_section_title
;
 3-(Dialkoxyphosphoryl)-N-confused Phlorin and Porphyrin. Synthesis,
 Stereochemistry, and Coordination Properties
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1354
_journal_page_last               1364
_journal_paper_doi               10.1021/jo302689d
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C52 H46 Cd Cl N4 O3 P'
_chemical_formula_sum            'C52 H46 Cd Cl N4 O3 P'
_chemical_formula_weight         953.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.692(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.9133(10)
_cell_length_b                   11.6762(4)
_cell_length_c                   31.8371(18)
_cell_measurement_reflns_used    6254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8079
_cell_measurement_theta_min      2.7370
_cell_volume                     10396.7(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            26730
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         11195
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+69.1570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                8081
_reflns_number_total             11195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302689d_si_003.cif
_cod_data_source_block           exp_863
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4027966