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_7227973
_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         'C16 H24 Na2 O15 P4 Zn2'
_chemical_formula_sum            'C16 H24 Na2 O15 P4 Zn2'
_chemical_formula_weight         756.95
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-12-17 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9501(18)
_cell_length_b                   5.2845(4)
_cell_length_c                   23.550(2)
_cell_measurement_reflns_used    1879
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.476
_cell_measurement_theta_min      2.682
_cell_volume                     2602.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.973
_diffrn_measured_fraction_theta_max 0.998
_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  0.0686
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6003
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         2.682
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.8615
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_meas      1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0389P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1616
_reflns_number_total             2293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00400a2.cif
_cod_data_source_block           1502888
_cod_original_cell_volume        2602.8(4)
_cod_database_code               7227973
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.656
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, All C(H,H) groups
 At 1.5 times of:
  H5 of O5, H8A of O8
2.a Riding coordinates:
 O7(H7)
2.b Rotating group:
 O8(H8A)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7A), C8(H8)
2.e Tetrahedral OH refined with riding coordinates:
 O5(H5)
;
_shelx_res_checksum              41114
_olex2_submission_special_instructions 'No special instructions were received'