Functionalized phosphonates as building units for multi-dimensional homo- and heterometallic 3d-4f inorganic-organic hybrid-materials.
Köhler, C; Rentschler, E.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12854–12861; doi:10.1039/c6dt02023b

data_7039947
_publ_section_title
;
 Functionalized phosphonates as building units for multi-dimensional homo-
 and heterometallic 3d-4f inorganic-organic hybrid-materials.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12854
_journal_page_last               12861
_journal_paper_doi               10.1039/c6dt02023b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C10 H16 N2 Ni O10 P2, 2.5(H2 O)'
_chemical_formula_sum            'C10 H21 N2 Ni O12.5 P2'
_chemical_formula_weight         489.94
_chemical_name_systematic        Compound-1b
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.491(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9582(16)
_cell_length_b                   10.0015(11)
_cell_length_c                   18.204(2)
_cell_measurement_reflns_used    1521
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.110
_cell_measurement_theta_min      2.322
_cell_volume                     1922.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.963
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0470 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.9227.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3098
_reflns_number_total             4605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02023b2.cif
_cod_data_source_block           Compound-1b
_cod_depositor_comments
'Adding full bibliography for 7039946--7039953.cif.'
_cod_original_cell_volume        1922.6(4)
_cod_original_formula_sum        'C10 H21 N2 Ni O12.50 P2'
_cod_database_code               7039947
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Sof(O12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(O12B)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5)
3.a Riding coordinates:
 O9(H9A,H9B)
3.b Free rotating group:
 O12B(H12A,H12B), O12A(H12C,H12D), O11(H11A,H11B), O13(H13A,H13B)
3.c Rotating group:
 O8(H8A,H8B), O10(H10A,H10B), O7(H7A,H7B)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C1(H1), C4(H4), C8(H8), C3(H3)
3.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O2(H2)
;
_shelx_res_checksum              62057
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'