Four new zinc (II) diphosphonates obtained via an ionothermal route: crystal structures and phase transformation behaviour
Zhang, Li; Li, Sanying; Liu, Lei; Dong, Jinxiang; Lin, Zhi; CrystEngComm  (2017) –; doi:10.1039/C7CE00400A

data_7227971
_publ_section_title
;
 Four new zinc (II) diphosphonates obtained via an ionothermal route:
 crystal structures and phase transformation behaviour
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00400A
_journal_year                    2017
_chemical_formula_moiety         '0.5(C16 H24 O16 P4 Zn4)'
_chemical_formula_sum            'C8 H12 O8 P2 Zn2'
_chemical_formula_weight         428.86
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-17 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.259(2)
_cell_length_b                   5.8452(6)
_cell_length_c                   4.9451(4)
_cell_measurement_reflns_used    1267
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.266
_cell_measurement_theta_min      3.662
_cell_volume                     643.40(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            2895
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         3.661
_exptl_absorpt_coefficient_mu    4.010
_exptl_absorpt_correction_T_max  0.8561
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.030(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.4595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                538
_reflns_number_total             607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00400a2.cif
_cod_data_source_block           1502886
_cod_database_code               7227971
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H3A(0.5) C4(0.5) H4(0.5)
3.a Riding coordinates:
 O3(H3), C1(H1A,H1B), C3(H3A), C4(H4)
;
_shelx_res_checksum              43970
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'