Stereoselective synthesis of the diazonamide a macrocyclic core.
Mutule, Ilga; Joo, Beomjun; Medne, Zane; Kalnins, Toms; Vedejs, Edwin; Suna, Edgars; The Journal of organic chemistry 80 (2015) 3058–3066; doi:10.1021/jo5029419

data_4030769
_publ_section_title
;
 Stereoselective synthesis of the diazonamide a macrocyclic core.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3058
_journal_page_last               3066
_journal_paper_doi               10.1021/jo5029419
_journal_volume                  80
_journal_year                    2015
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C36 H66 O2 P2 Pd, C4 H10 O1 '
_chemical_formula_sum            'C40 H76 O3 P2 Pd'
_chemical_formula_weight         773.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3194(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.61430(10)
_cell_length_b                   29.5816(4)
_cell_length_c                   13.6374(2)
_cell_measurement_reflns_used    10787
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      0.9
_cell_volume                     4236.92(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maXus(Mackay et al., 1999)'
_computing_structure_refinement  'maXus(Mackay et al., 1999)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.07419
_diffrn_orient_matrix_UB_12      0.03752
_diffrn_orient_matrix_UB_13      0.04640
_diffrn_orient_matrix_UB_21      -0.00422
_diffrn_orient_matrix_UB_22      -0.02906
_diffrn_orient_matrix_UB_23      0.01675
_diffrn_orient_matrix_UB_31      0.03668
_diffrn_orient_matrix_UB_32      0.02808
_diffrn_orient_matrix_UB_33      0.05795
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18649
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         28.5
_diffrn_reflns_theta_min         1.3
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.23
_refine_diff_density_rms         0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.389
_refine_ls_goodness_of_fit_gt    1.582
_refine_ls_goodness_of_fit_ref   1.528
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.097
_refine_ls_R_factor_gt           0.064
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details     ' w = 1 / ( s^2^(Fo^2^) + 0.10000 * Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.281
_refine_ls_wR_factor_gt          0.194
_refine_ls_wR_factor_ref         0.148
_reflns_d_resolution_high        0.61
_reflns_d_resolution_low         2.72
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                8267
_reflns_number_total             10845
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            jo5029419_si_002.cif
_cod_data_source_block           ZM598
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3086 2015-02-26 13:12:21Z robertas 

 Adding full bibliography for 4030769.cif.

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom, diff' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n        '
_cod_original_formula_sum        'C40 H76 O3 P2 Pd '
_cod_database_code               4030769