Crystal structure of aqua-bis(5-bromo-6-methyl-picolinato-κ2N,O)zinc(II) dihydrate, C14H16Br2N2O7Zn
Li, Jun-Xia; Du, Zhong-Xiang; Bai, Ruo-Fei; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 63–65; doi:10.1515/ncrs-2019-0486

data_8105018
_publ_section_title
;
 Crystal structure of aqua-bis(5-bromo-6-methyl-picolinato-\k2N,O)zinc(II)
 dihydrate, C14H16Br2N2O7Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              63
_journal_page_last               65
_journal_paper_doi               10.1515/ncrs-2019-0486
_journal_volume                  235
_journal_year                    2019
_chemical_absolute_configuration .
_chemical_formula_moiety         'C14 H12 Br2 N2 O5 Zn, 2(H2 O)'
_chemical_formula_sum            'C14 H16 Br2 N2 O7 Zn'
_chemical_formula_weight         549.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4300(3)
_cell_length_b                   10.6264(2)
_cell_length_c                   11.4638(2)
_cell_measurement_reflns_used    11531
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.4950
_cell_measurement_theta_min      3.7840
_cell_volume                     1879.67(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35861
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.758
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         3.554
_exptl_absorpt_coefficient_mu    5.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.432(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.4011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.720
_reflns_number_gt                3668
_reflns_number_total             4358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0486_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        1879.66(6)
_cod_database_code               8105018
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.568(11)
 0.432(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7D,H7E)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;