Tetracycline hydrochloride: a synchrotron micro-crystal study
Clegg, William; Teat, Simon J.; Acta Crystallographica Section C 56 (2000) 1343–1345; doi:10.1107/S0108270100010349

data_2011489
_publ_section_title
;
Tetracycline hydrochloride: a synchrotron micro-crystal study
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1343
_journal_page_last               1345
_journal_paper_doi               10.1107/S0108270100010349
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C22 H25 N2 O8 + , Cl -'
_chemical_formula_sum            'C22 H25 Cl N2 O8'
_chemical_formula_weight         480.89
_chemical_name_common            'tetracycline hydrochloride'
_chemical_name_systematic
;\
[(4S,4aS,5aS,6R,12aS)-2-aminohydroxymethylene-1,2,3,4,4a,5,5a,6,11,12a-\
decahydro-6,10,12,12a-tetrahydroxy-6-methyl-1,3,11-trioxonaphthacen-4-yl]\
dimethylammonium chloride
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9300(9)
_cell_length_b                   12.7162(11)
_cell_length_c                   15.7085(13)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      2.51
_cell_volume                     2183.3(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full .915
_diffrn_measured_fraction_theta_max .807
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer with Oxford Cryosystems open-flow cryostat
(Cosier & Glazer, 1986)
;
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     .6883
_diffrn_reflns_av_R_equivalents  .047
_diffrn_reflns_av_sigmaI/netI    .079
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8955
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          .04
_exptl_crystal_size_mid          .03
_exptl_crystal_size_min          .02
_refine_diff_density_max         .57
_refine_diff_density_min         -.24
_refine_ls_abs_structure_details 'Flack (1983); 1958 Friedel pairs'
_refine_ls_abs_structure_Flack   .02(8)
_refine_ls_extinction_coef       .0038(12)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1995)'
_refine_ls_goodness_of_fit_ref   .969
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .969
_refine_ls_R_factor_all          .063
_refine_ls_R_factor_gt           .050
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .116
_reflns_number_gt                3937
_reflns_number_total             4915
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1422Isup1.cif
_cod_data_source_block           I
_cod_database_code               2011489
_cod_database_fobs_code          2011489