Crystal structure of 4-bromo-2-(8-(3-ethoxy-2-hydroxyphenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenol, C18H19BrN2O5
Dong, Xiu-Yan; Liu, Jia-Cheng; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 805–807; doi:10.1515/ncrs-2015-0275

data_8107013
_publ_section_title
;
 Crystal structure of
 4-bromo-2-(8-(3-ethoxy-2-hydroxyphenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenol,
 C18H19BrN2O5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              805
_journal_page_last               807
_journal_paper_doi               10.1515/ncrs-2015-0275
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C18 H19 Br N2 O5'
_chemical_formula_sum            'C18 H19 Br N2 O5'
_chemical_formula_weight         423.26
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                70.954(11)
_cell_angle_beta                 84.794(8)
_cell_angle_gamma                72.691(8)
_cell_formula_units_Z            2
_cell_length_a                   9.0429(7)
_cell_length_b                   9.5752(11)
_cell_length_c                   11.8422(15)
_cell_measurement_reflns_used    1153
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      24.3470
_cell_measurement_theta_min      3.6270
_cell_volume                     925.34(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -12.00   19.50   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.8883  -99.0000  -60.0000 21

  2 omega  -66.00  -36.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.8883  120.0000  129.0000 20

  3 omega   -3.00   84.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       20.7321   38.0000  -30.0000 58

  4 omega   -7.00   89.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       20.7321   77.0000   60.0000 64

  5 omega  -48.00   63.00   1.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       20.7321  -19.0000  120.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0220807000
_diffrn_orient_matrix_UB_12      0.0639633000
_diffrn_orient_matrix_UB_13      0.0027672000
_diffrn_orient_matrix_UB_21      0.0086951000
_diffrn_orient_matrix_UB_22      -0.0332029000
_diffrn_orient_matrix_UB_23      0.0628882000
_diffrn_orient_matrix_UB_31      0.0786582000
_diffrn_orient_matrix_UB_32      -0.0385877000
_diffrn_orient_matrix_UB_33      -0.0072622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6052
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                2478
_reflns_number_total             3646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2015-0275_suppl.cif
_cod_data_source_block           D631
_cod_original_cell_volume        925.33(18)
_cod_database_code               8107013
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_olex2_date_sample_data_collection 2015-02-02
_olex2_submission_special_instructions 'No special instructions were received'