Two new ammonium/alkali-rare earth metal difluorophosphates ALa(PO<sub>2</sub>F<sub>2</sub>)<sub>4</sub> (A = NH<sub>4</sub> and K) with moderate birefringence and short cutoff edges.
Zhang, Wenyao; Wei, Zhonglei; Yang, Zhihua; Pan, Shilie; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11591–11596; doi:10.1039/d0dt01951h

data_7704932
_publ_section_title
;
 Two new ammonium/alkali-rare earth metal difluorophosphates
 ALa(PO<sub>2</sub>F<sub>2</sub>)<sub>4</sub> (A = NH<sub>4</sub> and K)
 with moderate birefringence and short cutoff edges.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11591
_journal_page_last               11596
_journal_paper_doi               10.1039/d0dt01951h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'F8 La O8 P4, H4 N'
_chemical_formula_sum            'F8 H4 La N O8 P4'
_chemical_formula_weight         560.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2020-07-12
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r1) 
;
_audit_update_record
;
2020-07-12 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.583(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.190(4)
_cell_length_b                   15.511(6)
_cell_length_c                   9.228(4)
_cell_measurement_reflns_used    3513
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.46
_cell_volume                     1397.9(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8510
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         2.464
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1182 before and 0.0476 after correction. 
The Ratio of minimum to maximum transmission is 0.6994. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5215
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0076(4)
_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   1.091
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+1.1861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2714
_reflns_number_total             3153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01951h2.cif
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi-scan ' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704931--7704932.cif.
;
_cod_original_cell_volume        1397.8(10)
_cod_database_code               7704932
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.560
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All N(H,H,H,H) groups 
2. Restrained distances 
 N1-H1A = N1-H1B = N1-H1C = N1-H1D 
 0.9 with sigma of 0.02 
 H1A-H1B = H1A-H1C = H1A-H1D = H1B-H1C = H1B-H1D = H1C-H1D 
 1.35 with sigma of 0.02 
 N1-H1A \\sim N1-H1B \\sim N1-H1C \\sim N1-H1D 
 with sigma of 0.02 
 H1A-H1B \\sim H1B-H1C \\sim H1C-H1D \\sim H1D-H1A \\sim H1B-H1D \\sim H1A-H1C 
 with sigma of 0.04 
3. Uiso/Uaniso restraints and constraints 
N1 \\sim H1A \\sim H1B \\sim H1C \\sim H1D: within 1.7A with sigma of 0.04 and 
sigma for terminal atoms of 0.08 
Uanis(F7) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.01 
Uanis(F8) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.004 
4. Rigid body (RIGU) restrains 
 N1, H1A, H1B, H1C, H1D 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 H1D, H1A, N1, H1B, H1C 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'